Effect of Chloride Content on Bond Behavior Between FRP and Concrete
海藻酸钠和氯化钙的作文
海藻酸钠和氯化钙的作文英文回答:Sodium alginate and calcium chloride are two commonly used chemicals in various industries. Sodium alginate, a compound derived from seaweed, is often used in food, pharmaceuticals, and even in textile printing. On the other hand, calcium chloride is a salt that is used for de-icing roads, in food preservation, and in the production of cheese.One interesting application of sodium alginate is in the creation of edible water bottles. By combining sodium alginate with calcium chloride, a gel-like substance is formed that can be molded into different shapes. This process, known as spherification, has been used by chefs to create unique culinary experiences. For example, a popular dessert called "spherical mango caviar" is made by dripping a mixture of mango juice and sodium alginate into a bath of calcium chloride, resulting in small, flavorful spheresthat burst in your mouth.In contrast, calcium chloride is commonly used in the food industry to preserve fruits and vegetables. It worksby inhibiting the growth of bacteria and mold, extendingthe shelf life of produce. For example, when making pickles, calcium chloride is added to the brine solution to ensure that the pickles stay crisp and fresh for longer periods of time.Overall, both sodium alginate and calcium chloride have unique properties that make them valuable in different industries. Whether it's creating edible water bottles or preserving fruits, these chemicals play a crucial role in our daily lives.中文回答:海藻酸钠和氯化钙是两种在各行各业中常用的化学物质。
陕产附子泡胆工艺的改进和优化研究
环球中医药2023年5月第16卷第5期 Global Traditional Chinese Medicine,May 2023,Vol.16,No.5867 ㊃中药研究㊃基金项目:陕西省科技计划项目(2020SF⁃325)作者单位:710003 西安,陕西省中医药研究院中药研究所(李凡㊁王卫锋㊁李莎莎㊁毛阿娟㊁李芳);西安国际医学中心有限公司药剂室(张景霞);陕西中医药大学药学院[李雅娟(硕士研究生)㊁陈曦(硕士研究生)]作者简介:李凡(1979-),硕士,助理研究员㊂研究方向:中药学㊂E⁃mail:15587646@通信作者:李芳(1973-),博士,主任药师,硕士生导师㊂研究方向:中药学㊂E⁃mail:527811472@陕产附子泡胆工艺的改进和优化研究李凡 张景霞 王卫锋 李莎莎 毛阿娟 李雅娟 陈曦 李芳【摘要】 目的 探讨氯化钙代替胆巴进行陕产附子泡胆的可能性和科学性,并对泡胆工艺参数进行优选㊂方法 以单/双酯型生物碱的含量为指标,进行胆巴溶液浸泡与氯化钙溶液浸泡陕产附子的泡胆工艺平行比较研究,然后以效/毒为评价指标,通过单因素试验结合Box⁃Behnken 响应面法,研究浸泡时间(分别浸泡6㊁12㊁18㊁24㊁30天,)㊁氯化钙浓度(分别加入浓度为10%㊁15%㊁20%㊁25%㊁30%的氯化钙溶液)㊁料液比(分别按料液比为1∶2㊁1∶3㊁1∶4㊁1∶5㊁1∶6加入25%的氯化钙溶液)对泡胆结果的影响,优选最佳泡胆工艺,并进行验证㊂结果 陕产附子分别经过较长时间的胆巴溶液㊁氯化钙溶液浸泡后生物碱总量均有所下降,且下降趋势一致㊂响应面最优工艺为:浸泡时间为19天㊁料液比为1∶4㊁氯化钙浓度为25%㊂验证试验中,平均效/毒为(0.069±0.012),在理论值0.071的误差范围内㊂结论 采用有药典标准的氯化钙代替胆巴作为附子防腐㊁加工和炮制的辅料㊂运用星点设计 效应面法,优选的陕产附子氯化钙泡胆工艺操作简便㊁稳定可靠,可为陕产附子的进一步炮制研究奠定基础㊂【关键词】 附子; 炮制; 胆巴; 氯化钙; 生物碱; Box⁃Behnken 响应面法【中图分类号】 R282.71 【文献标识码】 A doi:10.3969/j.issn.1674⁃1749.2023.05.008Research on the improvement and optimization of the brine soaking technology of Shaanxi ⁃produced crude aconiteLI Fan ,ZHANG Jingxia ,WANG Weifeng ,LI Shasha ,MAO Ajuan ,LI Yajuan ,CHEN Xi ,LI Fang Shaanxi Provincial Traditional Chinese Medicine Research Institute ,Xi ’an 710003,China Corresponding author :LI Fang ,E⁃mail :527811472@【Abstract 】 Objective Discuss the possibility and scientificity of calcium chloride instead of brineto soak Shaanxi ⁃produced crude aconite,and optimize the brine process parameters.Methods Taking thecontent of mono /diester alkaloids as the index,a parallel comparative study was carried out on the bilesoaking process of the aconite produced in Shaanxi province by soaking in bile solution and calcium chloride solution.Then using efficacy /toxicity as the evaluation index,the effects of soaking time(soakingfor 6,12,18,24,and 30days),calcium chloride concentration (adding 10%,15%,20%,25%,30%of calcium chloride),and material⁃to⁃liquid ratio (add 25%calcium chloride solution according to the material⁃to⁃liquid ratio of 1∶2,1∶3,1∶4,1∶5,1∶6respectively)on the soaking process were studied by the single factor test and Box⁃Behnken response surface methodology,and the soaking process was optimized and verified.Results The total amount of alkaloids of aconite produced in Shaanxi was decreased after being soaked in brine solution and calcium chloride solution for a long time,and the downward trend was consistent.The optimal soaking process was as follows:the soaking time was 19days,the material⁃to⁃liquid ratio was 1∶4,and the calcium chloride concentration was 25%.In the verification test,the average effect /toxicity was (0.069±0.012),which was within the error range of the theoreticalvalue of 0.071.Conclusion Calcium chloride with pharmacopoeia standards can be used instead of brine868 环球中医药2023年5月第16卷第5期 Global Traditional Chinese Medicine,May2023,Vol.16,No.5 as auxiliary materials for anti⁃corrosion and processing of crude ing the star⁃point design⁃response surface method,the optimized aconite calcium chloride soaking process is simple,stable andreliable,which can lay the foundation for the further research on aconite.【Key words】 Crude aconite; Processing technology; Brine; Calcium chloride; Alkaloids; Box⁃Behnken response surface methodology 附子为毛茛科植物乌头Aconitum carmichaelii Debx.的子根的加工品,始载于‘神农本草经“,味辛,甘,性大热,有毒㊂具有回阳救逆㊁补火助阳㊁散寒止痛之功[1]㊂附子为临床常用中药之一,陕西汉中是附子的原产区和主产区之一,种植历史悠久,产量大,并于2009年获得国家地理标志产品保护㊂附子作为毒性药材的代表,其炮制研究引起了广泛关注㊂自1963年起,附子在每版药典均有收载,多以炮制品入药,现代附子饮片市场主流为黑顺片等,现代部颁及药典标准方中运用的也有黑顺片等规格㊂法定标准中虽然对附子的炮制方法进行了规定,以黑顺片为例,炮制过程需经过泡胆㊁煮㊁浸漂㊁染色㊁蒸㊁晒(烘干)等环节,但其炮制工艺仍停留在传统的经验控制水平,没有明确的工艺参数,不同的操作者甚至同一操作者不同批次的加工,都无法保障黑顺片炮制加工工艺的稳定性及均一性,从而影响饮片的质量[2⁃3]㊂泡胆是黑顺片产地加工炮制的关键环节之一,胆巴的主要目的是为了防止附子腐烂,利于贮存㊂胆巴称卤水,是制盐工业的副产物,是老胆水经蒸发浓缩而凝固成型,其主要成分以氯化钙㊁氯化镁为主,能凝固蛋白质而具有防腐作用,对胃㊁皮肤㊁食管也具有腐蚀作用,而镁离子被吸收后能抑制心血管和神经系统,对人具有毒性[4],且胆巴无法定标准㊂本团队前期曾去陕西汉中实地考察,当地农户和企业有用氯化钙进行泡胆的操作㊂课题组采集了产自汉中4个县(区)的15批泥附子样品,采用超高效液相色谱法同时对样品中6种酯型生物碱的含量进行测定[5]㊂故本文在前期研究基础上拟对有药典标准的氯化钙代替传统胆巴作为附子防腐㊁加工和炮制的辅料的可能性和科学性进行探讨,并在单因素的基础上,以效/毒为指标,以三因素(浸泡时间㊁氯化钙浓度㊁料液比)三水平,采用Box⁃Behnken响应面设计对陕产附子的浸泡工艺进行优化㊂1 材料与方法1.1 实验材料附子(采于陕西汉中),样品经陕西省中医药研究院王卫锋教授鉴定均为毛茛科植物乌头(Aconitum carmichaelii Debx.)的子根;胆巴(四川省蓬莱盐化有限公司生产),氯化钙(食品级,山东海化股份有限公司氯化钙厂)㊂1.2 实验试剂对照品:苯甲酰新乌头原碱,批号:CHB180310,质量分数≥98%;苯甲酰乌头原碱,批号: CHB180309,质量分数≥98%;苯甲酰次乌头原碱,批号:CHB180307质量分数≥98%;乌头碱,批号: CHB180408,质量分数≥98%;新乌头碱,批号: CHB180311质量分数≥98%;次乌头碱,批号: CHB180524质量分数≥98%,均购自克洛玛科技有限公司㊂试剂:乙腈为HPLC级试剂(美国赛默飞公司),色谱用水(娃哈哈纯净水);其它试剂均为分析纯(国药集团)㊂1.3 实验仪器Waters Acquity H⁃CLASS型超高效液相色谱仪(UPLC EmpowerTM3色谱工作站㊁PDA检测器)㊁ACQUITY UPLC BEH C18色谱柱(2.1mm×50mm, 1.7μm)㊁电子分析天平(型号:BP211D型,德国赛多利斯)㊁超声波清洗机(型号:KH⁃300DE,昆山禾创超声仪器有限公司)㊁红外快速干燥箱(型号: WS70⁃1,上海市吴淞五金厂制造)㊁旋转蒸发仪(型号:RE⁃52AA,上海亚荣生化仪器厂)㊁循环水式多用真空泵(型号:SHB⁃III,郑州长城科工贸)㊁台式离心机(型号:TGL⁃16G,上海安亭科学)㊁电子调温电热套(型号:98⁃1⁃B,天津泰斯特)1.4 附子生物碱类成分的含量测定1.4.1 色谱条件与系统适用性实验 色谱柱为Waters ACQYITYC18柱(50mm×2.1mm,1.7μm);乙腈为流动相A,0.04mol/L乙酸铵溶液(氨水调pH=10)为流动相B,(A∶B,V∶V)0~5分钟, 26%A;5~15分钟,26%~39%A;15~20分钟,环球中医药2023年5月第16卷第5期 Global Traditional Chinese Medicine,May2023,Vol.16,No.586939%~45%A;20~25分钟,45%~39%A;25~30分钟,39%-26%A;流速:0.3mL/分钟;柱温: 25℃;对照品进样量:2μL;供试品进样体积:1μL;检测波长为235nm[6]㊂1.4.2 溶液的制备 (1)对照品溶液的制备:取苯甲酰新乌头原碱㊁苯甲酰乌头原碱㊁苯甲酰次乌头原碱㊁新乌头碱㊁乌头碱㊁次乌头碱对照品适量,精密称量,加异丙醇 二氯甲烷(1∶1)混合溶液,各质量浓度为:苯甲酰新乌头原碱46.36μg/mL㊁苯甲酰乌头原碱16.77μg/mL㊁苯甲酰次乌头原碱32. 105mg/mL㊁新乌头碱138.23μg/mL㊁乌头碱92.4μg/mL和次乌头碱130.82μg/mL㊂(2)供试品溶液的制备:取各个泡胆炮制环节的附子样品,洗净㊁切片后干燥,粉碎制备成粉末㊂取取各样品粉末(过三号筛)约2g,精密称定,置于锥形瓶中,加入氨试液3mL,精密加入异丙醇-乙酸乙酯(1∶1)混合溶液50mL,称重,超声处理(功率300W,频率40HZ,水温在25℃以下)30分钟,放冷,再称重,用异丙醇-乙酸乙酯(1∶1)混合溶液补足重量,摇匀,滤过,精密量取滤液25mL,40℃以下减压回收溶剂至干,精密加入0.05%盐酸甲醇溶液3mL复溶解残渣,过0.22μm滤膜,取滤液,即得[7]㊂1.5 泡胆工艺的改进1.5.1 胆巴溶液的配制 取胆巴加水配制成浓度为20%的胆巴溶液[8]㊂1.5.2 氯化钙溶液的配制 取氯化钙加水配制成浓度为20%的氯化钙溶液㊂1.5.3 不同浸泡时间考察 取附子约4kg,除去须根,洗净㊂分别取2kg,以1∶4的料液比浸入配制好的胆巴水溶液和氯化钙溶液中㊂浸泡时间均设定为:0天㊁1天㊁3天㊁5天㊁7天㊁9天㊁11天㊁13天㊁15天㊁16天㊁17天㊁18天㊁19天㊁20天㊁22天㊁25天㊁30天,分别浸泡不同时间后取出,纵切成厚约0.2~0.5cm的切片,在60°C下烘干,测定不同浸泡时间附子生物碱含量差别㊂2 结果2.1 附子生物碱类成分的含量测定超高效液相色谱法(UPLC)分别测定胆巴浸泡与氯化钙浸泡后双酯型(以乌头碱㊁新乌头碱㊁次乌头碱总量计)与单酯型(以苯甲酰新乌头原碱㊁苯甲酰乌头原碱㊁苯甲酰次乌头碱计)生物碱总量,测定结果见表1㊂附子经不同时间胆巴溶液与氯化钙溶液浸泡,双酯型生物碱总含量呈下降趋势㊂单酯型生物碱总量在浸泡第7天左右总量升高,在浸泡20天左右单酯型生物碱总量下降,处于平稳㊂实验结果得出,附子经过胆巴溶液与氯化钙溶液浸泡生物碱含量变化大体一致,产地加工可用氯化钙溶液浸泡附子代替胆巴溶液浸泡㊂结果见图1~2㊂表1 不同浸泡时间测定附子中生物碱含量浸泡时间(天)双酯型生物碱总量(mg/g)单酯型生物碱总量(mg/g)胆巴浸泡氯化钙浸泡胆巴浸泡氯化钙浸泡0 1.9353 1.97950.15190.14431 1.8620 1.82850.11870.1275 3 1.8022 1.81710.10710.1065 5 1.4750 1.41010.10920.1667 7 1.4546 1.44210.09500.0805 9 1.2548 1.01320.12160.0926 11 1.0602 1.09090.10310.1118 13 1.1019 1.06130.12310.1042 15 1.1159 1.00800.10290.9791 160.95020.97130.07330.0713 17 1.00990.92120.09170.0998 180.86610.84610.09520.0957 190.70700.70660.04030.0896 200.73570.79830.07790.0707 220.55840.53240.07390.0706 250.57190.52820.08100.0710 300.53080.49180.07440.0642图1 不同浸泡时间附子中双酯型生物碱总量变化趋势图870 环球中医药2023年5月第16卷第5期 Global Traditional Chinese Medicine,May2023,Vol.16,No.5图2 不同浸泡时间附子中单酯型生物碱总量变化趋势图2.2 改进后的泡胆工艺参数的优选2.2.1 单因素试验对泡胆初加工的考察 参考文献[8⁃10],在单因素试验中以效/毒值(苯甲酰新乌头原碱含量/双酯型生物碱总含量)为指标,可较为全面的反映附子在氯化钙水溶液中的浸泡过程,选取浸泡时间㊁氯化钙浓度㊁料液比为因素进行试验㊂2.2.2 浸泡时间对效/毒的影响 取附子,除须根,洗净,称取5份,每份约150g,按1∶4的料液比加入25%的氯化钙溶液,分别浸泡6㊁12㊁18㊁24㊁30天,切片,60°C下烘干㊂按本章 2.2.2”项下制备供试品,考察不同浸泡时间对效/毒的影响㊂可知,效/毒随着浸泡时间的增加,在18天时含量出现微下降㊂故选择浸泡时间为18天,结果见表2㊂2.2.3 料液比对效/毒的影响 取附子,除须根,洗净,称取5份,每份约150g,分别按料液比为1∶2㊁1∶3㊁1∶4㊁1∶5㊁1∶6加入25%的氯化钙溶液,浸泡18天,切片,60°C烘干㊂按本章 2.2.2”项下制备供试品,考察料液比对效/毒的影响㊂可知,效/毒随料液比的增加趋势趋于平缓,故选择料液比为1∶4,结果见表3㊂2.2.4 氯化钙浓度对效/毒的影响 取附子,除须根,洗净,称取5份,每份约150g,按料液比1∶4分别加入浓度为10%㊁15%㊁20%㊁25%㊁30%的氯化钙溶液,浸泡18天,切片㊁60°C下烘干㊂按本章 2.2.2”项下制备供试品,考察氯化钙用量对效/毒的影响㊂可知,随着氯化钙浓度的增加,效/毒在25%时最高㊂因此,选用25%的氯化钙溶液,结果见表4㊂2.2.5 Box⁃Behnken响应面法优选初加工工艺条件 在单因素试验基础上,采用中心组合设计,设计响应面试验,根据中心组合实验设计原理,用浸泡时间(X1)㊁料液比(X2)㊁氯化钙浓度(X3)为因素,以效/毒为响应值,结果见表5㊂表2 浸泡时间对附子效/毒的影响浸泡时间(天)称样量(g)指标成分(%)苯甲酰新乌头原碱新乌头碱乌头碱次乌头碱效/毒6 2.00520.00880.12500.05870.01690.044012 1.99970.00530.05090.01770.01360.064418 2.00450.00550.04050.01180.00510.096224 2.02350.00200.01410.00630.00200.090630 2.00140.00160.01040.00640.00510.0728表3 料液比对附子效/毒的影响料液比称样量(g)指标成分(%)苯甲酰新乌头原碱新乌头碱乌头碱次乌头碱效/毒1∶2 2.01560.00340.03250.01490.00390.0661 1∶3 2.00480.00310.02700.01220.00430.0705 1∶4 2.00020.00330.03050.01240.00410.0705 1∶5 2.01300.00390.03680.01200.00460.0704 1∶6 2.01110.00380.03770.01270.00520.0692环球中医药2023年5月第16卷第5期 Global Traditional Chinese Medicine,May2023,Vol.16,No.5871表4 氯化钙浓度对附子效/毒的影响氯化钙浓度(%)称样量(g)指标成分(%)苯甲酰新乌头原碱新乌头碱乌头碱次乌头碱效/毒10 2.00200.00310.04960.04090.00600.032315 2.00530.00220.03300.02510.00520.034120 2.01730.00250.03430.01140.00310.050225 2.00390.00260.02160.01540.00340.063130 2.01560.00270.02930.01520.00370.0563表5 响应面优化试验因素水平表因素水平-101浸泡时间(X1)12天18天24天料液比(X2)1∶31∶41∶5氯化钙浓度(X3)20%25%30% 2.3 响应面实验设计与结果2.3.1 响应面分析实验 通过浸泡时间(X1)㊁料液比(X2)㊁氯化钙浓度(X3)进行综合响应面分析,考察效/毒,结果见表6㊂表6 响应面分析实验设计与结果实验号浸泡时间(X1)料液比(X2)氯化钙浓度(X3)效/毒10000.0766 20000.0766 31010.0701 40000.0860 50-110.0526 61100.0587 701-10.0664 80000.0665 9-1010.0392 101-100.0571 110-1-10.0710 12-1100.0444 13-1-100.0495 140000.0769 1510-10.0544 16-10-10.0593 170110.0719 2.3.2 二次响应面回归模型建立 利用Design⁃Expert10.0.4软件,设计出不同的炮制工艺进行实验,以综合评分Y为响应值,分析得到回归方程为: Y=0.077+5.975E-003X1+1.382E-003X2-2.156 -003X3+1.692E-003X1X2+8.962E-003X1X3+5.960E-003X2X3-0.017X12-7.192E-003X22 -3.846E-003X32,相关系数R2=0.9077㊂2.3.3 二次响应面回归模型方差分析 从表7可以看出,模型的F=7.65,P=0.0069<0.01,表明此模型具有显著性,构建有效㊂失拟项P=7.78> 0.05,是不显著的,即试验数据和模型预测值相符合,模型构建合理㊂在本实验模型中,数据R2= 0.9077,Adj R2=0.78915,并且自变量和响应值之间有相互的对应关系,说明回归方程能够真实的模拟响应曲面的情况,响应值的变化有78.9%的概率与本实验考察的三因素变化有关㊂R2-Adj R2= 0.2,说明实验中存在的误差对实验结果影响不大㊂Adeq precisior=8.349,说明实验中存在的误差对实验结果影响也很小,信噪比很大,同时根据图4可以看出,预测值与实际值较近,本实验构建的模型能够预测效/毒值,由实验P值可知,本实验三个因素对效/毒的影响大小不同,顺序为X1>X3>X2,交互影响大小顺序为X1X3>X2X3>X1X2㊂其中X1㊁X1X3㊁X12㊁X22对综合评分较大(P<0.05),X2㊁X3㊁X1X2㊁X2 X3㊁X32影响较小(P>0.05)㊂2.3.4 响应面曲面分析 响应面坡度越陡,表示两因素交互作用越明显㊂等高线的形状可反映出交互效应的强弱大小,越密集,效应越强㊂椭圆形表示两因素交互作用显著,而圆形则相反㊂由图5㊁6㊁7可看出,AC和BC的等高线形成的椭圆形长轴和短轴之比较大,说明AC和BC之间交互影响比AB 之间交互影响显著㊂由图8可知,随着浸泡时间的增加,效/毒值也在增加,曲面变得陡峭,而料液比曲面相对平缓,说明浸泡时间影响较大㊂由图9可知,随着浸泡时间的增加,效/毒值先升高再降低,872 环球中医药2023年5月第16卷第5期 Global Traditional Chinese Medicine,May 2023,Vol.16,No.5曲面坡度较陡,而氯化钙浓度的增加,效/毒值曲面较平坦,相比来说浸泡时间的影响较大㊂由图10可知,在氯化钙浓度和料液比的增加,曲面走向变的平缓,根据3D 曲面图,得出浸泡时间和料液比,浸泡时间和氯化钙浓度的交互作用大于料液比和氯化钙的交互作用㊂经软件数据分析,响应面最优工艺为:X 1浸泡时间为19.2天㊁X 2料液比为1∶4.15㊁X 3氯化钙浓度为25.37%㊂2.3.5 验证试验 通过对图形数据的分析,对回归方程取一阶偏导数等于零,优化得到最佳的提取工艺为浸泡19.2天㊁料液比1∶4.15㊁氯化钙浓度25.37%㊂考虑实际条件,将浸泡时间㊁料液比及氯化钙浓度分别调整为19天㊁1∶4㊁25%㊂取生附子分为3份,用以上条件进行浸泡,得到平均效/毒为(0.069±0.012),在理论值0.071的误差范围内,说明回归模型建立得准确可靠㊂表7 响应面方差分析来源总偏差平方和自由度平均偏差平方和F 值P 值显著性模型 2.403E-0039 2.670E-0047.650.0069*X 1 2.856E-0041 2.856E-0048.180.0243*X 2 1.528E-0051 1.528E-0050.440.5293X 3 3.718E-0051 3.718E-005 1.070.3363X 1X 2 1.145E-0051 1.145E-0050.330.5848X 1X 3 3.213E-0041 3.213E-0049.210.0190*X 2X 3 1.421E-0041 1.421E-004 4.070.0834X 12 1.200E-0031 1.200E-00334.400.0006*X 22 2.178E-0041 2.178E-004 6.240.0411*X 32 6.228E-0051 6.228E-005 1.780.2234误差项 2.443E-0047 3.490E-005失拟项 5.227E-0053 1.742E-0050.360.7843绝对误差 1.920E-0044 4.800E-005所有项2.647E-00316图4 二次响应面回归构建的模型预测效/毒值与实际效/毒值比较图5 浸泡时间与料液比对附子效/毒的交互作用影响3D 图环球中医药2023年5月第16卷第5期 Global Traditional Chinese Medicine,May 2023,Vol.16,No.5873图6 浸泡时间与氯化钙浓度对附子效/毒的交互作用影响3D图图7 料液比与氯化钙浓度对附子效/毒的交互作用影响3D图图8 浸泡时间与料液比对附子效/毒的交互作用影响3D图图9 浸泡时间与氯化钙浓度对附子效/毒的交互作用影响3D图图10 氯化钙浓度与料液比对附子效/毒的交互作用影响3D 图3摇讨论通过二极管阵列检测器对样品在190nm ~400nm 进行扫描,结果在235nm 波长处,各色谱峰分离度较好,故选择235nm 作为检测波长㊂本实验通过查阅文献,分别考察了流动相系统:乙腈-0.04mol /L 乙酸铵㊁乙腈-0.1%甲酸水及乙腈-0.04mol /L 乙酸铵(调0.04mol /L 乙酸铵溶液的PH =10),结果以采用0.04mol /L 乙酸铵(PH =10)为流动相A,乙腈为流动相B 时各色谱峰能实现良好分离且基线平稳;考察了柱温对混合对照品分离效果的影响,结果得知在25℃㊁30℃㊁35℃的柱温下均比较稳定,对色谱峰的分离效果影响不明显,但考虑高柱温过高会对仪器和柱子可能造成损耗,最后将柱温设为25℃;最后考察了制样方法,首先考察了在制样过程中超声提取时加入氨试液对色谱峰的影响,其次考874 环球中医药2023年5月第16卷第5期 Global Traditional Chinese Medicine,May2023,Vol.16,No.5察了0.05%盐酸甲醇和异丙醇-二氯甲烷(1∶1复溶样品),最终确定的制样是需要加入氨试液,创造碱性环境,减压浓缩的残渣用0.05%盐酸甲醇复溶㊂本实验将附子分别在胆巴溶液和氯化钙溶液中浸泡20天时,与生附子相比,单酯和双酯型生物碱在胆巴中的降低率分别达到62%和51%;在氯化钙溶液中的降低率分别为60%和48%,之后两种溶液中含量趋于平缓,说明一定程度上氯化钙溶液浸泡附子可代替食用胆巴溶液浸泡,也证明了附子用胆腌足二十日”的记载[14]具有一定的合理性与科学性㊂有研究表明附子在胆巴溶液(以氯化钙计)中浸泡,在第9天到第25天时氯化钙含量逐渐增加,达到26%是到饱和状态,有防腐作用[15],与本实验优化的用25%的氯化钙溶液进行浸泡结果相符㊂本研究运用星点设计效应面法对改进后的陕产附子泡胆工艺进行了优选,为后期陕产附子的进一步炮制研究及质量控制研究等奠定了基础㊂参考文献[1] 国家药典委员会.中华人民共和国药典(一部)[M].北京:中国医药科技出版社,2020.[2] 杨洋,梅全喜,黄冉,等.中药附子炮制方法探讨[J].中国医院用药评价与分析,2021,21(4):505⁃507,512.[3] 凡若楠,张依欣,于武华,等.附子炮制的研究进展[J].江西中医药,2019,50(10):66⁃70.[4] 石万银.无胆附片加工工艺及其质量控制研究[D].成都:成都中医药大学,2012.[5] 李凡,田浩,马杰,等.陕西汉中不同产区泥附子中酯型生物碱类成分的测定[J].西北药学杂志,2022,37(2):6⁃10.[6] 汪云伟.基于化学成分及气味的附子(黑顺片)产地加工炮制过程研究[D].成都:成都中医药大学,2015. [7] 四川省食品药品监督管理局.四川省中药饮片炮制规范[M].成都:四川科学技术出版社,2015.[8] 杨千千.生附子等级标准与泡胆初加工工艺研究[D].杭州:浙江理工大学,2018.[9] 张定堃,韩雪,李瑞煜,等.UPLC⁃Q⁃TOF⁃MS分析不同产地附子化学成分的差异[J].中国中药杂志,2016,41(3):463⁃469.[10] 陈彦琳,杜杰,梁焕,等.道地药材附子炮制加工规范化探讨[J].中国现代中药,2009,11(7):42⁃44. [11] 丁璞,宋新,李先宽,等.星点及正交试验优化五味子藤茎提取工艺研究[J].中成药,2013,35(11):2534⁃2537. [12] 孙丽娜,杨源涛,王雪怡,等.响应面优化法在药学领域的应用[J].科技创新与应用,2017,(23):36⁃37. [13] 彭晓霞,路莎莎.响应面优化法在中药研究中的应用和发展[J].中国实验方剂学杂志,2011,17(19):296⁃299. [14] 董思含,孟江,吴孟华,等.附子历史沿革考辨[J].中国中药杂志,2020,45(22):5567⁃5575.[15] 周林,李飞,任玉珍,等.附子中胆巴含量随浸泡时间的变化趋势研究[J].中华中医药学刊,2013,31(11):2406⁃2408.(收稿日期:2022⁃05⁃10)(本文编辑:李梅)。
药物分析常用英语词汇
药物分析专业英语词汇表Aabsorbance 吸收度absorbance ratio 吸收度比值absorption 吸收absorption curve 吸收曲线absorption coefficient 吸收系数accurate value 准确值Acid—dye colormcty 酸性染料比色法acidimcty 酸量法acidity 酸度activity 活度adjusted retention time 调整保留时间absorbent 吸收剂absorption吸附alkalinity 碱度alumina 氧化铝,矾土ambient temperature 室温ammonium thiocyanate 硫氰酸铵analytical quality control 分析质量控制anhydrous substance 干燥品antioxidant 抗氧剂application of sample 点样area normalization method 面积归一法arsenic砷arsenic sport 砷斑assay 含量测定assay tolerance 含量限度attenuation 衰减acid burette 酸式滴定管alkali burette 碱式滴定管a mortar 研钵Bback extraction 反萃取band absorption 谱带吸收batch 批batch number 批号Benttendorlf method 白田道夫法between day precision 日间密度精biotransformation 生物转化blank test 空白试验boiling range 沸程British Pharmacopeia 英国药典bromate titration 溴酸盐滴定法bromine method 溴量法bromothymol blue 溴麝香酚蓝bulk drug 原料药by—product 副产物breaker 烧杯burette glass bead nozzle 滴定管brown acid burette 棕色酸式滴定管Ccalibration curve 校正曲线calomel electrode 甘汞电极calorimetry 量热分析capacity factor 容量因子capillary gas chromatography 毛细管气相色谱法carrier gas 载气characteristics description 性状chelate compound 螯合物chemical equivalent 化学当量Chinese pharmacopeia 中国药典Chinese material medicine 中成药Chinese material midical preparation 中药制剂chiral 手性的chiral carbon atom 手性碳原子chromatogram 色谱图chromatography 色谱法chromatographic column 色谱柱chromatographic condition 色谱条件clarity 澄清度coefficient of distribution 分配系数coefficient of variation 变异系数color change interval 变色范围color reaction 显色反应colormetry 比色法column efficiency 柱效column temperature 柱温comparative test 比较试验completeness of solution 溶液的澄清度conjugate 缀合物concentration—time curve 浓度时间曲线confidence interval 置信区间confidence level 置信水平controlled trial 对照试验correlation coefficient 相关系数contrast test 对照试验congealing point 凝点content unifarmity装量差异controlled trial 对照试验correlation coefficient 相关系数contrast test 对照试验counter ion 反离子cresal red 甲酚红cuvette cell 比色池cyanide氰化物casserole small 勺皿Ddead—stop titration 永定滴定法dead time 死时间deflection 偏差deflection point 拐点degassing 脱气deionized water 去离子水deliquescence 潮解depressor substances test 降压物质检查法desiccant 干燥剂detection 检查developing reagent 展开剂developing chamber 展开室deviation 偏差dextrose 右旋糖diastereoisomer 非对映异构体diazotization 重氮化differential thermal analysis 差示热分析法differential scanning calorimetry 差示扫描热法Gutzeit 古蔡day to day precision 日间精密度dissolution 溶出度direct injection 直接进样2,6-dichlorindophenol titration 2,6-二氯靛酚滴定法digestion 消化diphastic titration 双向滴定disintegration test 崩解试验dispersion 分散度dissolubility 溶解度dissolution test 溶解度检查distilling range 滴程distribution chromatography 分配色谱dose 剂量drug quality control 药品质量控制drying to constant weight 干燥至恒重duplicate test 重复试验disk method water method 压片法Eeffective constituent 有效成分effective plate number 有效板数effective of column 柱效electrophoresis 电泳elimination 消除eluate 洗脱液elution 洗脱enamtiomer 对映体end absorption 末端吸收endogenous substances 内源性物质enzyme drug 酶类药物enzyme induction 酶诱导enzyme inhibition 酶抑制epimer 差向异构体equilibrium constant 平衡常数error in volumetric analysis 容量分析误差exclusion chromatography 排阻色谱法expiration date 失效期external standard method 外标法extract 提取物extration gravimetry 提取重量法extraction titration 提取容量法extrapolated method外插法Erlenmeyer flask 锥形瓶evaporating dish small 蒸发皿elongated bulb 胖肚electronic balance MettlerAL204 MettlerAL204电子天平Ffactor 系数fehling's reaction 斐林实验filter 过滤fineness of the particles 颗粒细度flow rate 流速fluorescent agent 荧光剂fluorescence spectrophotometry 荧光分光光度法fluorescence detection 荧光检测器fluorescence analysis 荧光分析法foreign pigment 有色杂质formulary 处方集free 游离freezing test 冻结试验fused silica 熔融石英filter paper 滤纸Ggas chromatography 气相色谱法gas—liquid chromatography 气液色谱法gas purifier 气体净化器General identification test 一般鉴别试验general notices 凡例General requirements (药典)通则good clinical practices 药品临床管理规范good laboratory practices 药品实验室管理规范good manufacturing practices(GMP) 药品生产质量管理规范good supply practices(GSP) 药品供应管理规范gradient elution 梯度洗脱grating 光栅gravimetric method 重量法Gutzeit test 古蔡(检砷)法glass funnel long stem 玻璃漏斗grad cylinder 量筒glass rod 玻棒graduated pipettes 刻度吸管GC 气相色谱Hheavy metal 重金属half peak width 平峰宽heat conductivity 热导率height equivalent to a theoretical plate 理论塔板高度height of an effective plate 有效塔板高度high—performance liquid chromatography (HPLC)高效液相色谱法high—performance thin—layer chromatography (HPTLC)高效薄层色谱法hydrate 水合物hydrolysis 水解hydrophilicity 亲水性hydrophobicity 疏水性hydroxyl value 羟值hyperchromic effect 浓色效应hypochromic effect 淡色效应HHS-type constant temperature water bath HHS型恒温水锅HPLC 高效液相色谱法Iidentification 鉴别ignition to constant weight 灼烧至恒重immobile phase 固定相immunoassay 免疫测定impurity 杂质inactivation 失活index 索引indicator electrode 指示电极indicator 指示剂inhibitor 抑制剂injecting septum 进样隔膜胶垫instrumental analysis 仪器分析injection value 进样阀insulin assay 胰岛素生物检测法integrator 积分仪intercept 截距interface 接口internal standard substance 内标物质International unit 国际单位in vitro 体外in vivo 体内iodide 碘化物iodoform reation 碘仿反应iodometry 碘量法ion pair chromatography 离子对色谱ion suppression 离子抑制ion suppression 离子抑制ionic strength 离子强度ion—pairing agent 离子对试剂ionization 电离isoabsorptive point 等吸收点isocratic elution 等溶剂组成洗脱isoelectric point 等电点isoosmotic solution 等渗溶液irreversible indicator 不可逆指示剂irreversible potential 不可逆电位KKarl Fischer titration 卡尔—费舍尔滴定Kjeldahl method for nitrogen 凯氏定氮法Kober reagent 科伯试剂Kovats retention index 科瓦茨保留指数Llabelled amount 标示量leading peak 前延峰leveling effect 均化效应licensed pharmacist 执业药师limit control 限量控制limit of detection 检测限limit of quantitation 定量限limit test 杂质限度试验loss on drying 干燥失重low pressure gradient pump 氧压梯度泵linearity and range 线性及范围linearity scanning 线性扫描luminescence 发光litmus paper 石蕊试纸lyophilization 冷冻干燥Mmain constituent 主成分make—up gas 尾吹气maltol reaction 麦芽酚试验Marquis test 马奎斯试验mass analyzer detector 质量分析检测器mass spectrometric analysis 质谱分析mass spectrum 质谱图mean deviation 平均偏差melting point 熔点melting range 熔距metabolite 代谢物metastable ion 亚稳离子micellar chromatography 胶束色谱法microanalysis 微量分析microcrystal 微晶microdialysis 微透析migration time 迁移时间Millipore filtration 微孔过滤mobile phase 流动相molecular formula 分子式monitor 检测monochromator 单色器monographs 正文Nnatural product 天然产物Nessler’s reagent 碱性碘化汞试液neutralization 中和nitrogen content 总氮量nonaqueous acid—base titration 非水酸碱滴定nonprescription drug ,over the counter drugs 非处方药nonspecific impurity 一般杂质non-volatile matter 不挥发物normal phase 正相normalization 归一化法Nessler color comparison tube 纳氏比色管Onotice 凡例octadecyl silane bonded silicagel 十八烷基硅烷键合硅胶odorless 辛基硅烷odorless 无臭official name 法定名official test 法定试验on—column detector 柱上检测器on-column injection 柱头进样on the dried basis 按干燥品计opalescence 乳浊optical activity 光学活性optical isomerism 旋光异构optical purity 光学纯度organic volatile impurities 有机挥发性杂质orthogonal test 正交试验orthophenanthroline 邻二氮菲outlier 可疑数据overtones 倍频封oxidation-reduction titration 氧化还原滴定oxygen flask combustion 氧瓶燃烧Ppacked column 填充柱packing material 色谱柱填料palladium ion colorimetry 钯离子比色法parent ion 母离子particulate matter 不溶性微粒partition coefficient 分配系数pattern recognition(ppm)百万分之几peak symmetry 峰不对称性peak valley 峰谷peak width at half height 半峰宽percent transmittance 透光百分率pH indicator absorbance ratio method pH指示剂吸光度比值法pharmaceutical analysis 药物分析pharmacopeia 药典pharmacy 药学photometer 光度计polarimetry 旋光测定法polarity 极性polydextran gel 葡聚糖凝胶potentiometer 电位计potentiometric titration 电位滴定法precipitation form 沉淀形式precision 精密度preparation 制剂prescription drug 处方药pretreatment 预处理primary standard 基准物质principal component analysis 主成分分析prototype drug 原型药物purification 纯化purity 纯度pyrogen 热原pycnometer method 比重瓶法plastic wash bottle 洗瓶platform balance 天平pipette 移液管pyknowmeter flasks 容量瓶Qquality control 质量控制quality evaluation 质量评价quality standard 质量标准quantitative determination 定量测定quantitative analysis 定量分析quasi—molecular ion 准分子离子Rracemization 消旋化random sampling 随机抽样rational use of drug 合理用药readily carbonizable substance 易炭化物质reagent sprayer 试剂喷雾剂recovery 回收率reference electrode 参比电极related substance 相关物质relative density 相对密度relative intensity 相对强度repeatability 重复性replicate determination 平行测定reproducibility 重现性residual basic hydrolysis method 剩余碱水解法residual liquid junction potential 残余液接电位residual titration 剩余滴定residuce on ignition 炽灼残渣resolution 分辨率response time 响应时间retention 保留reversed phase chromatography 反相色谱法reverse osmosis 反渗透rinse 淋洗robustness 可靠性round 修约reagent bottles 试剂瓶round bottom flask 圆底烧瓶rubber suction bulb 洗耳球Ssafety 安全性Sakaguchi test 坂口试验salt bridge 盐桥salting out 盐析sample applicator 点样器sample application 点样sampling 取样saponification value 皂化值saturated calomel electrode 饱和甘汞电极selectivity 选择性significant difference 显著性水平significant testing 显著性检验silica get 硅胶silver chloride electrode 氯化银电极similarity 相似性sodium dodecylsulfate 十二基酸钠solid-phase extraction 固相萃取solubility 溶解度specific absorbance 吸收系数specification 规格specificity 专属性specific rotation 比旋度specific weight 比重spiked 加入标准的split injection 分流进样spray reagent 显色剂stability 稳定性standard color solution 标准比色液standard deviation 标准差standardization 标定standard substance 标准品statistical error 统计误差sterility test 无菌试验stock solution 储备液stoichiometric point 化学计量点storage 贮藏stray light 杂散光substrate 底物substituent 取代基sulfate 硫酸盐sulphated ash 硫酸盐灰分support 载体suspension 旋浊度swelling degree 膨胀度symmetry factor 对称因子systematic error 系统误差separating funnel 分液漏斗stopcock 玻璃活塞scissors 剪刀spirit lamp 酒精灯silica gel G thin layer 硅胶G薄层板Ttable 片剂tailing factor 拖尾因子tailing peak 拖尾峰test solution 试液thermal analysis 热分析法thermal conductivity detector 热导检测器thermogravimetric analysis 热重分析法The United States Pharmacopoeia 美国药典The Pharmacopoeia of Japan 日本药局方thin layer chromatography 薄层色谱thiochrome reaction 硫色素反应thymol 百里酚thymolphthalein 百里酚酞titer 滴定度three-dimensional chromatogram 三维色谱图titrant 滴定剂titration error 滴定误差titrimetric analysis 滴定分析法tolerance 容许限total ash 总灰分total quality control 全面质量控制traditional drugs 传统药traditional Chinese medicine 中药turbidance 浑浊turbidimetric assay 浊度测定法turbidimetry 比浊度turbidity 浊度Uultracentrifugation 超速离心ultraviolet irradiation 紫外线照射undue toxicity 异常毒性uniform design 均匀设计uniformity of dosage units 含量均匀度uniformity of volume 装量均匀性uniformity of weight 重量均匀性Vvalidity 可靠性variance 方差viscosity 粘度volatile oil determination apparatus 挥发油测定器volatilization 挥发性volumetric analysis 容量分析volumetric solution 滴定液volumetric flasks 比重瓶Wwave length 波长wave number 波数weighing bottle 称量瓶weighing form 称量形式well-closed container 密闭容器white board 白瓷板Xxylene cyanol blue FF 二甲苯蓝FF xylenol orange 二甲酚橙ZZigzag scanning 锯齿扫描zwitterions 两性离子Zymolysis 酶解作用zone electrophoresis 区带电泳。
偶氮二甲酰胺 氧化巯基 蛋白质
偶氮二甲酰胺氧化巯基蛋白质英文回答:The compound I want to discuss is called dithiothreitol (DTT), which is commonly used in biochemistry and molecular biology research. DTT is a reducing agent that is used to break disulfide bonds in proteins. It is also known as Cleland's reagent, named after the American biochemist William Cleland who first synthesized it.DTT is a white crystalline powder that is highlysoluble in water. It has a strong sulfur odor, which is characteristic of compounds containing thiol groups. DTT contains two thiol (-SH) groups, which are capable of forming covalent bonds with other molecules. When DTTreacts with proteins, it reduces the disulfide bonds (-S-S-) that hold the protein structure together. This process is known as reduction, and it results in the formation of two thiol groups.DTT is commonly used in protein biochemistry to denature proteins and to prevent protein aggregation. Denaturation is the process of unfolding a protein, which can be induced by heat or chemicals. By breaking the disulfide bonds, DTT helps to unfold the protein and expose its hydrophobic regions. This makes it easier to study the protein's structure and function.In addition to denaturation, DTT is also used to protect proteins from oxidation. Oxidation is a chemical reaction that can lead to the formation of reactive oxygen species, which can damage proteins and other biomolecules. By reducing the disulfide bonds, DTT prevents the formation of reactive oxygen species and protects the protein from oxidative damage.DTT is commonly used in a variety of experimental techniques, such as protein purification, protein folding studies, and enzyme assays. It is often added to protein samples or reaction mixtures at a final concentration of 1-10 mM. The exact concentration of DTT required depends on the specific experiment and the protein being studied.中文回答:英文回答:我要讨论的化合物叫做二硫苏糖醇(DTT),它在生物化学和分子生物学研究中常被使用。
共轭效应英文解释
共轭效应英文解释Conjugation is a chemical phenomenon that occurs in organic compounds when a series of atoms alternate double and single bonds. The presence of this alternation of bonds is known as the conjugated system, which gives rise to a phenomenon known as the conjugate effect.The conjugate effect is a chemical phenomenon that occurs when there is a transfer of electrons between conjugated double bonds located in a molecule. This transfer of electrons causes the electronic density in the molecule to redistribute, modifying its chemical properties, and giving rise to what is known as the conjugate effect.There are two types of conjugate effects: the +M effect and the -M effect. The +M effect, also known as the resonance effect, occurs when a group of atoms carries an odd number of electrons and has a lack of electrons that can be shared. This group of atoms tends to pull electrons towards itself, which creates a positive charge on the adjacent carbon atom.The -M effect, on the other hand, occurs when a group of atoms carries an even number of electrons and has an excessof electrons that can be shared. This group of atoms tends to push electrons away from itself, creating a negative charge on the adjacent carbon atom.The conjugate effect plays an essential role in determining the chemical properties of organic compounds. It affects the chemical reactivity, acidity, and basicity of organic molecules. For instance, the presence of a +M effect can enhance the reactivity of a molecule towards nucleophilesby providing increased electron density at the point of attack. Conversely, the presence of a -M effect can decrease reactivity towards electrophiles by decreasing electron density at positions susceptible to attack.In conclusion, the conjugate effect is an essential concept in organic chemistry that refers to theredistribution of electronic density in molecules. It results from the presence of conjugated double bonds in molecules and affects the chemical properties of organic compounds. The +M effect and the -M effect are two types of conjugate effects that have different effects on the electronic density in molecules. Understanding the conjugate effect is crucial for predicting the behavior of organic molecules in chemical reactions.。
异源表达棉花S-腺苷甲硫氨酸脱羧酶(GhSAMDC1)基因提高了拟南芥抗盐能力
Abstract: Transgenic Arabidopsis thaliana (GhSAMDC1) was used to study the effect of overexpression of GhSAMDC1 on salt tolerance of Arabidopsis thaliana seedlings, Contents of endogenous polyamines, hydrogen peroxide (H2O2), malondialdehyde (MDA), and chlorophyll, ion permeability, antioxidant enzymes (SOD, CAT, POD) activities and expression levels were investigated under salt stress. The overexpression of GhSAMDC1 decreased the content of endogenous putrescine (Put) and increased spermidine (Spd) and spermine (Spm) contents in Arabidopsis thaliana. Under salt stress, the expression levels of spermidine synthase (AtSPDS1, AtSPDS2) and spermine synthase (AtSPMS) in transgenic lines were significantly higher than those in wild type, the contents of Spd and Spm were further increased, and the contents of H2O2, MDA, chlorophyll, and ion permeability were obviously decreased. Compared with the wild type, Transgenic lines had no remarkable difference in peroxidase (POD) activity, but significantly higher superoxide dismutase (SOD) and catalase (CAT) activities, with the same change trend as their expression levels. Therefore, GhSAMDC1 increased the contents of Spd and Spm of transgenic plants by increasing the expression of genes related to Spd and Spm synthesis under salt stress, Spd and Spm directly or indirectly increased the activity of enzymes related to antioxidant system, and enhanced the salt tolerance of Arabidopsis thaliana by scavenging H2O2 and other reactive oxygen species. Keywords: Arabidopsis thaliana; cotton S-adenosylmethionine decarboxylase gene; salt stress; antioxidant enzyme
分析化学专业英语词汇总结
专业英语词汇-----分析化学第一章绪论分析化学:analytical chemistry定性分析:qualitative analysis定量分析:quantitative analysis物理分析:physical analysis物理化学分析:physico-chemical analysis仪器分析法:instrumental analysis流动注射分析法:flow injection analysis;FIA顺序注射分析法:sequentical injection analysis;SIA化学计量学:chemometrics第二章误差的分析数据处理绝对误差:absolute error相对误差:relative error系统误差:systematic error可定误差:determinate error随机误差:accidental error不可定误差:indeterminate error准确度:accuracy精确度:precision偏差:debiation,d平均偏差:average debiation相对平均偏差:relative average debiation标准偏差(标准差):standerd deviation;S相对平均偏差:relatibe standard deviation;RSD变异系数:coefficient of variation误差传递:propagation of error有效数字:significant figure置信水平:confidence level显著性水平:level of significance合并标准偏差(组合标准差):pooled standard debiation 舍弃商:rejection quotient ;Q化学定量分析第三章滴定分析概论滴定分析法:titrametric analysis滴定:titration容量分析法:volumetric analysis化学计量点:stoichiometric point等当点:equivalent point电荷平衡:charge balance电荷平衡式:charge balance equation质量平衡:mass balance物料平衡:material balance质量平衡式:mass balance equation第四章酸碱滴定法酸碱滴定法:acid-base titrations 质子自递反应:auto protolysis reaction质子自递常数:autoprotolysis constant质子条件式:proton balance equation酸碱指示剂:acid-base indicator指示剂常数:indicator constant变色范围:colour change interval混合指示剂:mixed indicator双指示剂滴定法:double indicator titration第五章非水滴定法非水滴定法:nonaqueous titrations质子溶剂:protonic solvent酸性溶剂:acid solvent碱性溶剂:basic solvent两性溶剂:amphototeric solvent无质子溶剂:aprotic solvent均化效应:differentiatin g effect区分性溶剂:differentiating solvent离子化:ionization离解:dissociation结晶紫:crystal violet萘酚苯甲醇: α-naphthalphenol benzyl alcohol奎哪啶红:quinadinered百里酚蓝:thymol blue偶氮紫:azo violet溴酚蓝:bromophenol blue第六章配位滴定法配位滴定法:compleximetry乙二胺四乙酸:ethylenediamine tetraacetic acid,EDTA 螯合物:chelate compound金属指示剂:metal lochrome indcator第七章氧化还原滴定法氧化还原滴定法:oxidation-reduction titration碘量法:iodimetry溴量法:bromimetry ]溴量法:bromine method铈量法:cerimetry高锰酸钾法:potassium permanganate method条件电位:conditional potential溴酸钾法:potassium bromate method硫酸铈法:cerium sulphate method偏高碘酸:metaperiodic acid高碘酸盐:periodate亚硝酸钠法:sodium nitrite method重氮化反应:diazotization reaction重氮化滴定法:diazotization titration亚硝基化反应:nitrozation reaction亚硝基化滴定法:nitrozation titration外指示剂:external indicator外指示剂:outside indicator重铬酸钾法:potassium dichromate method 第八章沉淀滴定法沉淀滴定法:precipitation titration容量滴定法:volumetric precipitation method 银量法:argentometric method第九章重量分析法重量分析法:gravimetric analysis挥发法:volatilization method引湿水(湿存水):water of hydroscopicity 包埋(藏)水:occluded water吸入水:water of imbibition结晶水:water of crystallization组成水:water of composition液-液萃取法:liquid-liquid extration溶剂萃取法:solvent extration反萃取:counter extraction分配系数:partition coefficient分配比:distribution ratio离子对(离子缔合物):ion pair沉淀形式:precipitation forms称量形式:weighing forms仪器分析概述物理分析:physical analysis物理化学分析:physicochemical analysis仪器分析:instrumental analysis第十章电位法及永停滴定法电化学分析:electrochemical analysis电解法:electrolytic analysis method电重量法:electrogravimetry库仑法:coulo metry库仑滴定法:coulo metric titration电导法:conductometry电导分析法:conductometric analysis电导滴定法:conductometric titration电位法:potentiometry直接电位法:dirext potentiometry电位滴定法:potentiometric titration伏安法:voltammetry极谱法:polarography溶出法:stripping method电流滴定法:amperometric titration化学双电层:chemical double layer相界电位:phase boundary potential 金属电极电位:electrode potential化学电池:chemical cell液接界面:liquid junction boundary原电池:galvanic cell电解池:electrolytic cell负极:cathode正极:anode电池电动势:eletromotive force指示电极:indicator electrode参比电极:reference electroade标准氢电极:standard hydrogen electrode一级参比电极:primary reference electrode饱和甘汞电极:saturated calomel electrode银-氯化银电极:silver silver-chloride electrode液接界面:liquid junction boundary不对称电位:asymmetry potential表观PH值:apparent PH复合PH电极:combination PH electrode离子选择电极:ion selective electrode敏感器:sensor晶体电极:crystalline electrodes均相膜电极:homogeneous membrance electrodes非均相膜电极:heterogeneous membrance electrodes非晶体电极:non- crystalline electrodes刚性基质电极:rigid matrix electrode流流体载动电极:electrode with a mobile carrier气敏电极:gas sensing electrodes酶电极:enzyme electrodes金属氧化物半导体场效应晶体管:MOSFET离子选择场效应管:ISFET总离子强度调节缓冲剂:total ion strength adjustment buffer,TISAB永停滴定法:dead-stop titration双电流滴定法(双安培滴定法):double amperometric titration 第十一章光谱分析法概论普朗克常数:Plank constant电磁波谱:electromagnetic spectrum光谱:spectrum光谱分析法:spectroscopic analysis原子发射光谱法:atomic emission spectroscopy质量谱:mass spectrum质谱法:mass spectroscopy,MS第十二章紫外-可见分光光度法紫外-可见分光光度法:ultraviolet and visible spectrophotometry;UV-vis肩峰:shoulder peak末端吸收:end absorbtion生色团:chromophore助色团:auxochrome红移:red shift长移:bathochromic shift短移:hypsochromic shift蓝(紫)移:blue shift增色效应(浓色效应):hyperchromic effect减色效应(淡色效应):hypochromic effect强带:strong band弱带:weak band吸收带:absorption band透光率:transmitance,T吸光度:absorbance谱带宽度:band width杂散光:stray light噪声:noise暗噪声:dark noise散粒噪声:signal shot noise闪耀光栅:blazed grating全息光栅:holographic grating光二极管阵列检测器:photodiode array detector 偏最小二乘法:partial least squares method ,PLS褶合光谱法:convolution spectrometry褶合变换:convolution transform,CT离散小波变换:wavelet transform,WT多尺度细化分析:multiscale analysis供电子取代基:electron donating group吸电子取代基:electron with-drawing group第十三章荧光分析法荧光:fluorescence荧光分析法:fluorometryX-射线荧光分析法:X-ray fluorometry原子荧光分析法:atomic fluorometry分子荧光分析法:molecular fluorometry振动弛豫:vibrational relaxation内转换:internal conversion外转换:external conversion体系间跨越:intersystem crossing激发光谱:excitation spectrum荧光光谱:fluorescence spectrum斯托克斯位移:Stokes shift荧光寿命:fluorescence life time荧光效率:fluorescence efficiency荧光量子产率:fluorescence quantum yield荧光熄灭法:fluorescence quenching method散射光:scattering light瑞利光:R a yleith scattering light拉曼光:Raman scattering lightAbbe refractometer 阿贝折射仪absorbance 吸收度absorbance ratio 吸收度比值absorption 吸收absorption curve 吸收曲线absorption spectrum 吸收光谱absorptivity 吸收系数accuracy 准确度acid-dye colorimetry 酸性染料比色法acidimetry 酸量法acid-insoluble ash 酸不溶性灰分acidity 酸度activity 活度第十四章色谱法additive 添加剂additivity 加和性adjusted retention time 调整保留时间adsorbent 吸附剂adsorption 吸附affinity chromatography 亲和色谱法aliquot (一)份alkalinity 碱度alumina 氧化铝ambient temperature 室温ammonium thiocyanate 硫氰酸铵analytical quality control(AQC)分析质量控制anhydrous substance 干燥品anionic surfactant titration 阴离子表面活性剂滴定法antibiotics-microbial test 抗生素微生物检定法antioxidant 抗氧剂appendix 附录application of sample 点样area normalization method 面积归一化法argentimetry 银量法arsenic 砷arsenic stain 砷斑ascending development 上行展开ash-free filter paper 无灰滤纸(定量滤纸)assay 含量测定assay tolerance 含量限度atmospheric pressure ionization(API) 大气压离子化attenuation 衰减back extraction 反萃取back titration 回滴法bacterial endotoxins test 细菌内毒素检查法band absorption 谱带吸收baseline correction 基线校正baseline drift 基线漂移batch, lot 批batch(lot) number 批号Benttendorff method 白田道夫(检砷)法between day (day to day, inter-day) precision 日间精密度between run (inter-run) precision 批间精密度biotransformation 生物转化bioavailability test 生物利用度试验bioequivalence test 生物等效试验biopharmaceutical analysis 体内药物分析,生物药物分析blank test 空白试验boiling range 沸程British Pharmacopeia (BP) 英国药典bromate titration 溴酸盐滴定法bromimetry 溴量法bromocresol green 溴甲酚绿bromocresol purple 溴甲酚紫bromophenol blue 溴酚蓝bromothymol blue 溴麝香草酚蓝bulk drug, pharmaceutical product 原料药buret 滴定管by-product 副产物calibration curve 校正曲线calomel electrode 甘汞电极calorimetry 量热分析capacity factor 容量因子capillary zone electrophoresis (CZE) 毛细管区带电泳capillary gas chromatography 毛细管气相色谱法carrier gas 载气cation-exchange resin 阳离子交换树脂ceri(o)metry 铈量法characteristics, description 性状check valve 单向阀chemical shift 化学位移chelate compound 鳌合物chemically bonded phase 化学键合相chemical equivalent 化学当量Chinese Pharmacopeia (ChP) 中国药典Chinese material medicine 中成药Chinese materia medica 中药学Chinese materia medica preparation 中药制剂Chinese Pharmaceutical Association (CPA) 中国药学会chiral 手性的chiral stationary phase (CSP) 手性固定相chiral separation 手性分离chirality 手性chiral carbon atom 手性碳原子chromatogram 色谱图chromatography 色谱法chromatographic column 色谱柱chromatographic condition 色谱条件chromatographic data processor 色谱数据处理机chromatographic work station 色谱工作站clarity 澄清度clathrate, inclusion compound 包合物clearance 清除率clinical pharmacy 临床药学coefficient of distribution 分配系数coefficient of variation 变异系数color change interval (指示剂)变色范围color reaction 显色反应colorimetric analysis 比色分析colorimetry 比色法column capacity 柱容量column dead volume 柱死体积column efficiency 柱效column interstitial volume 柱隙体积column outlet pressure 柱出口压column temperature 柱温column pressure 柱压column volume 柱体积column overload 柱超载column switching 柱切换committee of drug evaluation 药品审评委员会comparative test 比较试验completeness of solution 溶液的澄清度compound medicines 复方药computer-aided pharmaceutical analysis 计算机辅助药物分析concentration-time curve 浓度-时间曲线confidence interval 置信区间confidence level 置信水平confidence limit 置信限congealing point 凝点congo red 刚果红(指示剂)content uniformity 装量差异controlled trial 对照试验correlation coefficient 相关系数contrast test 对照试验counter ion 反离子(平衡离子)cresol red 甲酚红(指示剂)crucible 坩埚crude drug 生药crystal violet 结晶紫(指示剂)cuvette, cell 比色池cyanide 氰化物cyclodextrin 环糊精cylinder, graduate cylinder, measuring cylinder 量筒cylinder-plate assay 管碟测定法daughter ion (质谱)子离子dead space 死体积dead-stop titration 永停滴定法dead time 死时间decolorization 脱色decomposition point 分解点deflection 偏差deflection point 拐点degassing 脱气deionized water 去离子水deliquescence 潮解depressor substances test 降压物质检查法derivative spectrophotometry 导数分光光度法derivatization 衍生化descending development 下行展开desiccant 干燥剂detection 检查detector 检测器developer, developing reagent 展开剂developing chamber 展开室deviation 偏差dextrose 右旋糖,葡萄糖diastereoisomer 非对映异构体diazotization 重氮化2,6-dichlorindophenol titration 2,6-二氯靛酚滴定法differential scanning calorimetry (DSC) 差示扫描热量法differential spectrophotometry 差示分光光度法differential thermal analysis (DTA) 差示热分析differentiating solvent 区分性溶剂diffusion 扩散digestion 消化diphastic titration 双相滴定disintegration test 崩解试验dispersion 分散度dissolubility 溶解度dissolution test 溶出度检查distilling range 馏程distribution chromatography 分配色谱distribution coefficient 分配系数dose 剂量drug control institutions 药检机构drug quality control 药品质量控制drug release 药物释放度drug standard 药品标准drying to constant weight 干燥至恒重dual wavelength spectrophotometry 双波长分光光度法duplicate test 重复试验effective constituent 有效成分effective plate number 有效板数efficiency of column 柱效electron capture detector 电子捕获检测器electron impact ionization 电子轰击离子化electrophoresis 电泳electrospray interface 电喷雾接口electromigration injection 电迁移进样elimination 消除eluate 洗脱液elution 洗脱emission spectrochemical analysis 发射光谱分析enantiomer 对映体end absorption 末端吸收end point correction 终点校正endogenous substances 内源性物质enzyme immunoassay(EIA) 酶免疫分析enzyme drug 酶类药物enzyme induction 酶诱导enzyme inhibition 酶抑制eosin sodium 曙红钠(指示剂)epimer 差向异构体equilibrium constant 平衡常数equivalence point 等当点error in volumetric analysis 容量分析误差excitation spectrum 激发光谱exclusion chromatography 排阻色谱法expiration date 失效期external standard method 外标法extract 提取物extraction gravimetry 提取重量法extraction titration 提取容量法extrapolated method 外插法,外推法factor 系数,因数,因子feature 特征Fehling’s reaction 费林反应field disorption ionization 场解吸离子化field ionization 场致离子化filter 过滤,滤光片filtration 过滤fineness of the particles 颗粒细度flame ionization detector(FID) 火焰离子化检测器flame emission spectrum 火焰发射光谱flask 烧瓶flow cell 流通池flow injection analysis 流动注射分析flow rate 流速fluorescamine 荧胺fluorescence immunoassay(FIA) 荧光免疫分析fluorescence polarization immunoassay(FPIA) 荧光偏振免疫分析fluorescent agent 荧光剂fluorescence spectrophotometry 荧光分光光度法fluorescence detection 荧光检测器fluorimetyr 荧光分析法foreign odor 异臭foreign pigment 有色杂质formulary 处方集fraction 馏分freezing test 结冻试验funnel 漏斗fused peaks, overlapped peaks 重叠峰fused silica 熔融石英gas chromatography(GC) 气相色谱法gas-liquid chromatography(GLC) 气液色谱法gas purifier 气体净化器gel filtration chromatography 凝胶过滤色谱法gel permeation chromatography 凝胶渗透色谱法general identification test 一般鉴别试验general notices (药典)凡例general requirements (药典)通则good clinical practices(GCP) 药品临床管理规范good laboratory practices(GLP) 药品实验室管理规范good manufacturing practices(GMP) 药品生产质量管理规范good supply practices(GSP) 药品供应管理规范gradient elution 梯度洗脱grating 光栅gravimetric method 重量法Gutzeit test 古蔡(检砷)法half peak width 半峰宽[halide] disk method, wafer method, pellet method 压片法head-space concentrating injector 顶空浓缩进样器heavy metal 重金属heat conductivity 热导率height equivalent to a theoretical plate 理论塔板高度height of an effective plate 有效塔板高度high-performance liquid chromatography (HPLC) 高效液相色谱法high-performance thin-layer chromatography (HPTLC) 高效薄层色谱法hydrate 水合物hydrolysis 水解hydrophilicity 亲水性hydrophobicity 疏水性hydroscopic 吸湿的hydroxyl value 羟值hyperchromic effect 浓色效应hypochromic effect 淡色效应identification 鉴别ignition to constant weight 灼烧至恒重immobile phase 固定相immunoassay 免疫测定impurity 杂质inactivation 失活index 索引indicator 指示剂indicator electrode 指示电极inhibitor 抑制剂injecting septum 进样隔膜胶垫injection valve 进样阀instrumental analysis 仪器分析insulin assay 胰岛素生物检定法integrator 积分仪intercept 截距interface 接口interference filter 干涉滤光片intermediate 中间体internal standard substance 内标物质international unit(IU) 国际单位in vitro 体外in vivo 体内iodide 碘化物iodoform reaction 碘仿反应iodometry 碘量法ion-exchange cellulose 离子交换纤维素ion pair chromatography 离子对色谱ion suppression 离子抑制ionic strength 离子强度ion-pairing agent 离子对试剂ionization 电离,离子化ionization region 离子化区irreversible indicator 不可逆指示剂irreversible potential 不可逆电位isoabsorptive point 等吸收点isocratic elution 等溶剂组成洗脱isoelectric point 等电点isoosmotic solution 等渗溶液isotherm 等温线Karl Fischer titration 卡尔·费歇尔滴定kinematic viscosity 运动黏度Kjeldahl method for nitrogen 凯氏定氮法Kober reagent 科伯试剂Kovats retention index 科瓦茨保留指数labelled amount 标示量leading peak 前延峰least square method 最小二乘法leveling effect 均化效应licensed pharmacist 执业药师limit control 限量控制limit of detection(LOD) 检测限limit of quantitation(LOQ) 定量限limit test (杂质)限度(或限量)试验limutus amebocyte lysate(LAL) 鲎试验linearity and range 线性及范围linearity scanning 线性扫描liquid chromatograph/mass spectrometer (LC/MS) 液质联用仪litmus paper 石蕊试纸loss on drying 干燥失重low pressure gradient pump 低压梯度泵luminescence 发光lyophilization 冷冻干燥main constituent 主成分make-up gas 尾吹气maltol reaction 麦牙酚试验Marquis test 马奎斯试验mass analyzer detector 质量分析检测器mass spectrometric analysis 质谱分析mass spectrum 质谱图mean deviation 平均偏差measuring flask, volumetric flask 量瓶measuring pipet(te) 刻度吸量管medicinal herb 草药melting point 熔点melting range 熔距metabolite 代谢物metastable ion 亚稳离子methyl orange 甲基橙methyl red 甲基红micellar chromatography 胶束色谱法micellar electrokinetic capillary chromatography(MECC, MEKC) 胶束电动毛细管色谱法micelle 胶束microanalysis 微量分析microcrystal 微晶microdialysis 微透析micropacked column 微型填充柱microsome 微粒体microsyringe 微量注射器migration time 迁移时间millipore filtration 微孔过滤minimum fill 最低装量mobile phase 流动相modifier 改性剂,调节剂molecular formula 分子式monitor 检测,监测monochromator 单色器monographs 正文mortar 研钵moving belt interface 传送带接口multidimensional detection 多维检测multiple linear regression 多元线性回归multivariate calibration 多元校正natural product 天然产物Nessler glasses(tube) 奈斯勒比色管Nessler’s r eagent 碱性碘化汞钾试液neutralization 中和nitrogen content 总氮量nonaqueous acid-base titration 非水酸碱滴定nonprescription drug, over the counter drugs (OTC drugs) 非处方药nonproprietary name, generic name 非专有名nonspecific impurity 一般杂质non-volatile matter 不挥发物normal phase 正相normalization 归一化法notice 凡例nujol mull method 石蜡糊法octadecylsilane chemically bonded silica 十八烷基硅烷键合硅胶octylsilane 辛(烷)基硅烷odorless 无臭official name 法定名official specifications 法定标准official test 法定试验on-column detector 柱上检测器on-column injection 柱头进样on-line degasser 在线脱气设备on the dried basis 按干燥品计opalescence 乳浊open tubular column 开管色谱柱optical activity 光学活性optical isomerism 旋光异构optical purity 光学纯度optimization function 优化函数organic volatile impurities 有机挥发性杂质orthogonal function spectrophotometry 正交函数分光光度法orthogonal test 正交试验orthophenanthroline 邻二氮菲outlier 可疑数据,逸出值overtones 倍频峰,泛频峰oxidation-reduction titration 氧化还原滴定oxygen flask combustion 氧瓶燃烧packed column 填充柱packing material 色谱柱填料palladium ion colorimetry 钯离子比色法parallel analysis 平行分析parent ion 母离子particulate matter 不溶性微粒partition coefficient 分配系数parts per million (ppm) 百万分之几pattern recognition 模式识别peak symmetry 峰不对称性peak valley 峰谷peak width at half height 半峰宽percent transmittance 透光百分率pH indicator absorbance ratio method? pH指示剂吸光度比值法pharmaceutical analysis 药物分析pharmacopeia 药典pharmacy 药学phenolphthalein 酚酞photodiode array detector(DAD) 光电二极管阵列检测器photometer 光度计pipeclay triangle 泥三角pipet(te) 吸移管,精密量取planar chromatography 平板色谱法plate storage rack 薄层板贮箱polarimeter 旋光计polarimetry 旋光测定法polarity 极性polyacrylamide gel 聚丙酰胺凝胶polydextran gel 葡聚糖凝胶polystyrene gel 聚苯乙烯凝胶polystyrene film 聚苯乙烯薄膜porous polymer beads 高分子多孔小球post-column derivatization 柱后衍生化potentiometer 电位计potentiometric titration 电位滴定法precipitation form 沉淀形式precision 精密度pre-column derivatization 柱前衍生化preparation 制剂prescription drug 处方药pretreatment 预处理primary standard 基准物质principal component analysis 主成分分析programmed temperature gas chromatography 程序升温气相色谱法prototype drug 原型药物provisions for new drug approval 新药审批办法purification 纯化purity 纯度pyrogen 热原pycnometric method 比重瓶法quality control(QC) 质量控制quality evaluation 质量评价quality standard 质量标准quantitative determination 定量测定quantitative analysis 定量分析quasi-molecular ion 准分子离子racemization 消旋化radioimmunoassay 放射免疫分析法random sampling 随机抽样rational use of drug 合理用药readily carbonizable substance 易炭化物reagent sprayer 试剂喷雾器recovery 回收率reference electrode 参比电极refractive index 折光指数related substance 有关物质relative density 相对密度relative intensity 相对强度repeatability 重复性replicate determination 平行测定reproducibility 重现性residual basic hydrolysis method 剩余碱水解法residual liquid junction potential 残余液接电位residual titration 剩余滴定residue on ignition 炽灼残渣resolution 分辨率,分离度response time 响应时间retention 保留reversed phase chromatography 反相色谱法reverse osmosis 反渗透rider peak 驼峰rinse 清洗,淋洗robustness 可靠性,稳定性routine analysis 常规分析round 修约(数字)ruggedness 耐用性safety 安全性Sakaguchi test 坂口试验salt bridge 盐桥salting out 盐析sample applicator 点样器sample application 点样sample on-line pretreatment 试样在线预处理sampling 取样saponification value 皂化值saturated calomel electrode(SCE) 饱和甘汞电极selectivity 选择性separatory funnel 分液漏斗shoulder peak 肩峰signal to noise ratio 信噪比significant difference 显著性差异significant figure 有效数字significant level 显著性水平significant testing 显著性检验silanophilic interaction 亲硅羟基作用silica gel 硅胶silver chloride electrode 氯化银电极similarity 相似性simultaneous equations method 解线性方程组法size exclusion chromatography(SEC) 空间排阻色谱法sodium dodecylsulfate, SDS 十二烷基硫酸钠sodium hexanesulfonate 己烷磺酸钠sodium taurocholate 牛璜胆酸钠sodium tetraphenylborate 四苯硼钠sodium thiosulphate 硫代硫酸钠solid-phase extraction 固相萃取solubility 溶解度solvent front 溶剂前沿solvophobic interaction 疏溶剂作用specific absorbance 吸收系数specification 规格specificity 专属性specific rotation 比旋度specific weight 比重spiked 加入标准的split injection 分流进样splitless injection 无分流进样spray reagent (平板色谱中的)显色剂spreader 铺板机stability 稳定性standard color solution 标准比色液standard deviation 标准差standardization 标定standard operating procedure(SOP) 标准操作规程standard substance 标准品stationary phase coating 固定相涂布starch indicator 淀粉指示剂statistical error 统计误差sterility test 无菌试验stirring bar 搅拌棒stock solution 储备液stoichiometric point 化学计量点storage 贮藏stray light 杂散光substituent 取代基substrate 底物sulfate 硫酸盐sulphated ash 硫酸盐灰分supercritical fluid chromatography(SFC) 超临界流体色谱法support 载体(担体)suspension 悬浊液swelling degree 膨胀度symmetry factor 对称因子syringe pump 注射泵systematic error 系统误差system model 系统模型system suitability 系统适用性tablet 片剂tailing factor 拖尾因子tailing peak 拖尾峰tailing-suppressing reagent 扫尾剂test of hypothesis 假设检验test solution(TS) 试液tetrazolium colorimetry 四氮唑比色法therapeutic drug monitoring(TDM) 治疗药物监测thermal analysis 热分析法thermal conductivity detector 热导检测器thermocouple detector 热电偶检测器thermogravimetric analysis(TGA) 热重分析法thermospray interface 热喷雾接口The United States Pharmacopoeia(USP) 美国药典The Pharmacopoeia of Japan(JP) 日本药局方thin layer chromatography(TLC) 薄层色谱法thiochrome reaction 硫色素反应three-dimensional chromatogram 三维色谱图thymol 百里酚(麝香草酚)(指示剂)thymolphthalein 百里酚酞(麝香草酚酞)(指示剂)thymolsulfonphthalein ( thymol blue) 百里酚蓝(麝香草酚蓝)(指示剂)titer, titre 滴定度time-resolved fluoroimmunoassay 时间分辨荧光免疫法titrant 滴定剂titration error 滴定误差titrimetric analysis 滴定分析法tolerance 容许限toluene distillation method 甲苯蒸馏法toluidine blue 甲苯胺蓝(指示剂)total ash 总灰分total quality control(TQC) 全面质量控制traditional drugs 传统药traditional Chinese medicine 中药transfer pipet 移液管turbidance 混浊turbidimetric assay 浊度测定法turbidimetry 比浊法turbidity 浊度ultracentrifugation 超速离心ultrasonic mixer 超生混合器ultraviolet irradiation 紫外线照射undue toxicity 异常毒性uniform design 均匀设计uniformity of dosage units 含量均匀度uniformity of volume 装量均匀性(装量差异)uniformity of weight 重量均匀性(片重差异)validity 可靠性variance 方差versus …对…,…与…的关系曲线viscosity 粘度volatile oil determination apparatus 挥发油测定器volatilization 挥发法volumetric analysis 容量分析volumetric solution(VS) 滴定液vortex mixer 涡旋混合器watch glass 表面皿wave length 波长wave number 波数weighing bottle 称量瓶weighing form 称量形式weights 砝码well-closed container 密闭容器xylene cyanol blue FF 二甲苯蓝FF(指示剂)xylenol orange 二甲酚橙(指示剂)zigzag scanning 锯齿扫描zone electrophoresis 区带电泳zwitterions 两性离子zymolysis 酶解作用簡體書目錄Chapter 1 Introduction 緒論1.1 The nature of analytical chemistry 分析化學的性質1.2 The role of analytical chemistry 分析化學的作用1.3 The classification of analytical chemistry分析化學的分類1.4 The total analytical process分析全過程Terms to understand重點內容概述Chapter 2 Errors and Data Treatment in Quantitative Analysis 定量分析中的誤差及數據處理2.1 Fundamental terms of errors誤差的基本術語2.2 Types of errors in experimental data實驗數據中的誤差類型2.2.1 Systematic errors 系統誤差2.2.2 Random errors偶然誤差2.3 Evaluation of analytical data分析數據的評價2.3.1 Tests of significance顯著性檢驗2.3.2 Rejecting data可疑值取捨2.4 Significant figures有效數字ProblemsTerms to understand重點內容概述Chapter 3 Titrimetric Analysis滴定分析法3.1 General principles基本原理3.1.1 Relevant terms of titrimetric analysis滴定分析相關術語3.1.2 The preparation of standard solution and the expression of concentration 標準溶液的配製與濃度表示方法3.1.3 The types of titrimetric reactions滴定反應類型3.2 Acid-base titration酸鹼滴定3.2.1 Acid-base equilibria 酸鹼平衡3.2.2 Titration curves滴定曲線3.2.3 Acid-base indicators酸鹼指示劑3.2.4 Applications of acid-base titration酸鹼滴定的應用3.3 Complexometric titration配位滴定3.3.1 Metal-chelate complexes金屬螯合物3.3.2 EDTA 乙二胺四乙酸3.3.3 EDTA titration curves EDTA滴定曲線3.3.4 Metal Ion indicators金屬離子指示劑3.3.5 Applications of EDTA titration techniques EDTA滴定方法的應用3.4 Oxidation-reduction titration氧化還原滴定3.4.1 Redox reactions氧化還原反應3.4.2 Rate of redox reactions氧化還原反應的速率3.4.3 Titration curves滴定曲線3.4.4 Redox indicators氧化還原指示劑3.4.5 Applications of redox titrations氧化還原滴定的應用3.5 Precipitation titration沉澱滴定3.5.1 Precipitation reactions沉澱滴定反應3.5.2 Titration curves滴定曲線3.5.3 End-point detection終點檢測ProblemsTerms to understand重點內容概述Chapter 4 Potentiometry 電位分析法4.1 Introduction簡介4.1.1 Classes and characteristics分類及性質4.1.2 Definition定義4.2 Types of potentiometric electrodes電極種類4.2.1 Reference electrodes 參比電極4.2.2 Indicator electrodes指示電極4.2.3 Electrode response and selectivity電極響應及選擇性4.3 Potentiometric methods and application電位法及應用4.3.1 Direct potentiometric measurement 直接電位法4.3.2 Potentiometric titrations電位滴定4.3.3 Applications of potentiometry 電位法應用ProblemsTerlns to understand重點內容概述Chapter 5 Chromatography色譜法5.1 An introduction to chromatographic methods色譜法概述5.2 Fundamental theory of gas chromatography氣相色譜基本原理5.2.1 Plate theory塔板理論5.2.2 Kinetic theory(rate theory) 速率理論5.2.3 The resolution Rs as a measure of peak separation 分離度5.3 Gas chromatography 氣相色譜5.3.1 Components of a gas chromatograph 氣相色譜儀的組成5.3.2 Stationary phases for gas-liquid chromatography 氣液色譜固定相5.3.3 Applications of gas-liquid chromatography 氣液色譜的應用5.3.4 Adsorption chromatography 吸附色譜5.4 High performance liquid chromatography 高效液相色譜5.4.1 Instrumentation 儀器組成5.4.2 High-performance partition chromatography 高效分配色譜5.5 Miscellaneous separation methods 其他分離方法5.5.1 High-performance ion-exchange chromatography 高效離子交換色譜5.5.2 Capillary electrophoresis 毛細管電泳5.5.3 Planar chromatography 平板色譜ProblemsTerms to understand重點內容概述Chapter 6 Atomic Absorption Spectrometry原子吸收光譜分析法6.1 Introduction 概述6.2 Principles 原理6.2.1 The process of AAS,resonance line and absorption line 原子吸收光譜法的過程,共振線及吸收線6.2.2 The number of ground atom and the temperature of flame 基態原子數與光焰溫度6.2.3 Quantitative analysis of AAS原子吸收光譜定量分析6.3 Instrumentation 儀器6.3.1 Primary radiation sources 光源6.3.2 Atomizer 原子儀器6.3.3 Optical dispersive systems 分光系統6.3.4 Detectors 檢測器6.3.5 Signal measurements 信號測量6.4 Quantitative measurements and interferences 定量測定及干擾6.4.1 Quantitative measurements 定量測定6.4.2 Interferences 干擾6.4.3 Sensitivity6.5 Applications of AAS原子吸收光譜法的應用ProblemsTerms to understand重點內容概述Chapter 7 Ultraviolet and Visible Spectrophotometry 紫外-可見分光光度法7.1 Introduction簡介7.2 Ultraviolet and visible absorption spectroscopy 紫外-可見吸收光譜7.2.1 Introduction for radiant energy 輻射能簡介7.2.2 Selective absorption of radiation and absorbance spectrum 物質對光的選擇性吸收和吸收光譜7.2.3 Absorbing species and electron transition 吸收物質與電子躍遷7.3 Law of absorption吸收定律7.3.1 Lambert-Beer's law朗伯-比爾定律7.3.2 Absorptivity吸光係數7.3.3 Apparent deviations from Beer's law對比爾定律的明顯偏離7.4 Instruments儀器7.5 General types of spectrophotometer分光光度計種類7.6 Application of UV-Vis absorption spectroscopy 紫外-可見吸收光譜的應用7.6.1 Application of absorption measurement to qualitative analysis 光吸收測定在定性分析上的應用7.6.2 Quantitative analysis by absorption measurements 光吸收測量定量分析法7.6.3 Derivative spectrophotometry 導數分光光度法ProblemsTerms to understand重點內容概述Chapter 8 Infrared Absorption Spectroscopy紅外吸收光譜8.1 Theory of infrared absorption紅外吸收基本原理8.1.1 Dipole changes during vibrations and rotations 振轉運動中的偶極距變化8.1.2 Mechanical model of stretching vibrations 伸縮振動機械模型8.1.3 Quantum treatment of vibrations 振動的量子力學處理、8.1.4 Types of molecular vibrations分子振動形式8.2 Infrared instrument components紅外儀器組成8.2.1 Wavelength selection波長選擇8.2.2 Sampling techniques 採樣技術8.2.3 Infrared spectrophotometers for qualitative analysis 定性分析用紅外分光光度計8.2.4 Other techniques其他技術8.3 The group frequencies of functional groups in organic compounds 有機化合物官能團的特徵頻率8.4 The factors affecting group frequencies 影響基團特徵吸收頻率的因素8.4.1 Adjacent groups 鄰近基團的影響。
槲皮素与酪蛋白和牛血清白蛋白的相互作用及共存碳纳米管的影响
槲皮素与酪蛋白和牛血清白蛋白的相互作用及共存碳纳米管的影响陈代武;谢青季;蒋雪琴;姚守拙【期刊名称】《物理化学学报》【年(卷),期】2008(24)3【摘要】Fluorescence quenching and synchronous fluorescence methods were used to study the interactions of fluorescence'activequercetin(Qct)with casein(Cas)and bovine serum albumin(BSA)in phosphate buffer solution(PBS,pH=7.4)with or without coexisting carbon nanotubes(CNTs).Formulae for binding constant(k)and molarrnbindingratio(n)wereestablishedformethodsl(fLxingproteinconcentra tion,changingQctconcentration,andmonitoring the fluorescence of protein)and 2(fixing Qct concentration,changing protein concentration。
And monitoring the fluorescence ofQct),towhich values ofKand,1were calculated via nonfinearleast-squarefitting of the experimental data,and the"optical inner filtering induced fluorescence quenching"effect WaS thus quantitatively evaluated.The quenching effects ofcoexisting CNTs on the fluorescence of Qct,BSA,and Cas。
外源CaCl2对盐胁迫下棉花种子萌发及幼苗叶片抗氧化酶活性的影响
绿洲农业科学与工程Oasis Agriculture Science and Engineering第9卷第2期2023年12月Vol.9No.2Dec.2023棉花(Gossypium hirsutum L.)是我国重要的经济作物。
我国棉花的生产量、消费量位居世界前列[1]。
新疆是全国最大的产棉区,产量占全国棉花总产量60%以上,棉花生产在新疆经济发展中占有收稿日期:2022-10-31基金项目:国家自然科学基金(41461064)作者简介:李国钰(2001-),女,甘肃天水人,硕士研究生,研究方向为植物抗逆生理。
E-mail :*****************通讯作者:张淑英(1976-),女,新疆克拉玛依人,副教授,研究方向为植物营养及植物逆境生理研究。
E-mail :**************************外源CaCl 2对盐胁迫下棉花种子萌发及幼苗叶片抗氧化酶活性的影响李国钰,张淑英*,程恩俊(石河子大学农学院,新疆石河子832003)摘要:为探究盐胁迫下氯化钙(CaCl 2)引发对棉花种子萌发、幼苗生长及叶片抗氧化酶活性的影响,以棉花品种“天云0769”为供试材料,采用纸上萌发处理,研究不同浓度CaCl 2(0、10、20、30、40、50mmol·L -1浸种后,在150mmol·L -1盐(NaCl )胁迫下,棉花种子萌发指标(GP 、GR 、GI 、VI )、幼苗生物量、电解质渗出率及抗氧化酶(SOD 、POD 、CAT 和APX )活性的影响。
研究表明,在150mmol·L -1NaCl 胁迫下,棉花种子萌发指标(GP 、GR 、GI 、VI )、棉花幼苗干、鲜重及抗氧化酶(SOD 、POD 、CAT 和APX )活性均较CK 显著下降(P<0.05),电解质渗出率升高;CaCl 2浸种处理后,随CaCl 2浓度升高棉花种子萌发指标(GP 、GR 、GI 、VI )、幼苗干、鲜重及抗氧化酶(SOD 、POD 、CAT 和APX )活性均呈先升后降趋势,电解质渗出率呈先降后升的趋势。
等渗盐胁迫下Na+和Cl-对大豆幼苗光合作用的离子效应
等渗盐胁迫下Na+和Cl-对大豆幼苗光合作用的离子效应陈宣钦;於丙军【期刊名称】《植物生理与分子生物学学报》【年(卷),期】2007(033)004【摘要】Ion-specific stress effects of Na+ and Cl- on photosynthesis of seedlings of two soybean (Glycine max) isoosmotic (-0.53 MPa) solutions [PEG-6000, NaCl, Na+ (without Cl-) and Cl- (without Na+)] for 6 d. The results showed that the chlorophyll contents and the ribulose bisphosphate carboxylase/oxygenase (Rubisco) activities of seedlings of both cultivars were inhibited to a less degree by PEG-6000 than by NaCl, Na+ (without Cl-) or Cl- (without Na+) solutions. The maximum photochemical efficiency of photosystem Ⅱ (PSⅡ) (Fv/Fm), electron transfer rate (ETR) and effective quantum yield of PSⅡ photochemistry (Fv'/Fm') were lowered significantly by PEG-6000 treatment for 2 d and 6 d. But when treated with the three isoosmotic salt stresses, most of the above three indexes significantly declined. Leaf stomatal conductance (Gs) and net photosynthetic rate (Pn) in both cultivars were significantly decreased under the four isoosmotic treatments, and much more drops were observed in the three salt stresses, but the intercellular CO2 concentration (Ci) decreased by PEG-6000 treatment and increased by the three salt stresses. Higher decreases including chlorophyll content, Rubisco activity, Fv/Fm,ETR, Fv'/Fm', Pn and Gs, and higher contents of Cl- as well as thecontent of Cl- plus Na+ in chloroplasts were all observed under Cl- (without Na+) treatment than those under Na+ (without Cl-) treatment, especially for the saltamong the adverse effects of NaCl stress on photosynthesis of G. max seedlings, the ionic toxicity was stronger than osmotic stress, and the toxicity of Cl- was more severe than that of Na+.%研究和比较了等渗(-0.53 MPa)的PEG-6000、NaCl、钠盐(无Cl-)和氯化物(无Na+)溶液处理6 d对栽培大豆品种'Lee68'(耐盐性较强)和'N23674'(耐盐性较弱)幼苗光合作用的离子效应.结果表明:PEG-6000处理使两品种叶片叶绿素含量和Rubisco活性较对照低,但降幅不如同样渗透压的NaCl、钠盐(无Cl-)和氯化物(无Na+)溶液明显.PSⅡ最大光化学效率(Fv/Fm)、电子传递速率(ETR)和PSⅡ光化学的有效量子产额(Fv'/Fm')在PEG-6000处理2 d和6 d时显著下降,但在3种等渗盐处理下,多显著下降.两品种叶片气孔导度(Gs)和净光合速率(Pn)在4种胁迫处理下均显著下降,其中在3种盐处理下更明显,但胞间CO2浓度(Ci)仅在PEG-6000处理时下降,在盐处理下反而升高.两品种叶片叶绿素含量、Rubisco活性、Fv/Fm、ETR、Fv'/Fm'、Pn、Gs等在氯化物(无Na+)溶液处理的下降幅度和叶绿体中Cl-含量及其与Na+总量的增加幅度均大于钠盐(无Cl-)处理的,在耐盐性弱的'N23674'品种中更明显.可见,在NaCl胁迫对栽培大豆幼苗光合作用的毒害效应中,渗透胁迫较轻,离子毒害较重,其中Cl-的毒害大于Na+的.【总页数】7页(P294-300)【作者】陈宣钦;於丙军【作者单位】南京农业大学,生命科学学院,南京,210095;南京农业大学,生命科学学院,南京,210095;南京农业大学,大豆研究所农业部国家大豆改良中心,南京,210095【正文语种】中文【中图分类】Q945【相关文献】1.盐胁迫下外源脯氨酸对甜瓜幼苗体内K+、Na+、Ca2+、Mg2+和Cl-含量及分布的影响 [J], 颜志明;魏跃;胡德龙;王全智;郭世荣2.NaCl胁迫下Cl-和Na+对大豆幼苗胁迫作用的比较 [J], 罗庆云;於丙军;刘友良3.盐胁迫下Na+、K+和Cl-对碱蓬和玉米生理特性效应的比较研究 [J], 贾洪涛;高文;刘京贞;战祥强4.盐胁迫下氯丙嗪和LaCl3对稻苗K+、Na+、Cl-吸收转运的影响 [J], 宗会;徐照丽;刘娥娥;李明启5.盐胁迫下Na+,K+,Cl—对碱蓬和玉米离子的吸收效应 [J], 贾洪涛;赵可夫因版权原因,仅展示原文概要,查看原文内容请购买。
复合酶法提取槐花多糖的工艺优化及其抗氧化活性
任晓莉,杨璐,乔鹏,等. 复合酶法提取槐花多糖的工艺优化及其抗氧化活性[J]. 食品工业科技,2024,45(7):8−14. doi:10.13386/j.issn1002-0306.2023070216REN Xiaoli, YANG Lu, QIAO Peng, et al. Optimization of Extraction Process of Polysaccharide from Sophora japonica by Compound Enzyme Method and Its Antioxidant Activity[J]. Science and Technology of Food Industry, 2024, 45(7): 8−14. (in Chinese with English abstract). doi: 10.13386/j.issn1002-0306.2023070216· 特邀主编专栏—食品中天然产物提取分离、结构表征和生物活性(客座主编:杨栩、彭鑫) ·复合酶法提取槐花多糖的工艺优化及其抗氧化活性任晓莉*,杨 璐,乔 鹏,缪奕锴,杨懿昂,代秋红,张贤德(太原工业学院环境与安全工程系,山西太原 030008)摘 要:目的:采用复合酶法提取槐花多糖,对提取工艺进行优化,并评价其体外抗氧化活性。
方法:通过单因素实验考察复合酶添加量、pH 、复合酶比例和酶解时间对得率的影响,在单因素实验基础上,采用响应面法确定槐花多糖的最佳提取参数,并以V C 为对照,通过测定槐花多糖对DPPH·和ABTS +·的清除率及总还原力,考察所提取的槐花多糖的抗氧化活性。
结果:复合酶法提取槐花多糖的最佳提取参数为:复合酶添加量23.8 mg/g ,pH4.8,果胶酶与纤维素酶比例0.912:1,该工艺下槐花多糖得率为10.71%,所提取的槐花多糖对DPPH·和ABTS +·均表现出较好的清除能力,当槐花多糖溶液浓度为2.8 mg/mL 时,对DPPH·和ABTS +·的清除率分别达到同浓度下V C 的94.19%和99.79%,总还原力达到V C 的75.99%。
pH值和缓冲剂对抗坏血酸_半胱氨酸模式反应形成香味化合物的影响
pH 值和缓冲剂对抗坏血酸-半胱氨酸模式反应形成香味化合物的影响刘应煊,余爱农(湖北民族学院化学与环境工程学院,湖北 恩施 445000)摘 要:以固相微萃取-气相色谱-质谱联用技术对抗坏血酸与半胱氨酸的模式反应产物进行鉴定,研究pH 值和缓冲剂浓度对模式反应形成香味化合物的影响。
依赖于不同的p H 值条件,模式反应主要产生呋喃、吡嗪、噻唑、噻吩及含硫脂环化合物,这些化合物种类及产量的变化形成各具特色的肉香风味,呋喃类化合物主要形成于低pH 值条件下,而吡嗪类化合物则易于在碱性条件下生成,噻唑类化合物的形成与p H 值的依赖性不太显著,但过高的酸度会抑制其生成,中性偏碱的条件对噻吩和含硫脂环化合物的生成有利;Na 2HPO 4-NaH 2PO 4缓冲剂对模式反应没有催化作用,它们对模式反应形成香味化合物的影响体现于其维持反应体系pH 值稳定的能力,0.20mol/L Na 2HPO 4-NaH 2PO 4缓冲剂对维持反应体系pH 值的相对稳定是合适的。
关键词:M ai l l ar d 反应;抗坏血酸;香味化合物;固相微萃取;p H 值;缓冲剂Effect of pH and Buffer on Aroma Compound Generation from Model Reaction of Ascorbic Acid with CysteineLIU Ying-xuan ,YU Ai-nong(School of Chemical and Environmental Engineering, Hubei University for Nationalities, Enshi 445000, China)Abstract :The aroma compounds generated from a model reaction system of ascorbic acid (ASA) and cysteine (Cys) were identified by solid-phase microextraction-gas chromatography-mass spectrometry (SPME-GC-MS). The effects of pH and buffer concentration on the formation of aroma compounds were investigated. The major aroma compounds including furans,pyrazines, thiazoles, thiophenes, and alicyclic S compounds were generated in the model reaction system at various pH conditions. The types and amounts of these compounds could result in the formation of distinctive meat-like flavor. Furans were produced mainly under acidic pH conditions. In contrast, pyrazines were easy to generate in an alkaline environment. Thiazoles formation was not affected by pH, but high acidity could inhibit their generation. Neutral or slightly alkaline medium was conducive to the formation of thiophenes and alicyclic S compounds. Na 2HPO 4-NaH 2PO 4 buffer did not exhibit catalytic effect on the model reaction; on the other hand, its effect on aroma compound generation from model reaction system was exclusively concentrated on the ability to keep the pH stable. Therefore, 0.20 mol/L Na 2HPO 4-NaH 2PO 4 buffer is appropriate to maintain a relatively stable pH in the model reaction system.Key words :Maillard reaction ;ascorbic acid ;aroma compound ;solid-phase microextraction ;pH ;buffer 中图分类号:TS201.7 文献标识码:A 文章编号:1002-6630(2012)06-0143-07收稿日期:2011-03-08基金项目:国家自然科学基金面上项目(20876036)作者简介:刘应煊(1977—),男,讲师,硕士,主要从事气相色谱-质谱联用技术研究。
CTAB对多巴胺和抗坏血酸电分析的影响
中文摘要本实验研究的是多巴胺和抗坏血酸在与阳离子表面活性剂CTAB(十六烷基三甲基溴化铵)的共存体系中的电化学性质。
从实验中发现,CTAB对于多巴胺有很大的影响,它减弱了多巴胺的氧化和还原反应,从而给出了一个与没有CATB时相对较小的非均相速率常数,k0,诱发该过程趋于不可逆转。
与此相反,对于抗坏血酸来说,氧化反应却得到了加强。
这些效果可以影响多巴胺和抗坏血酸伏安信号的分离直到453 mV。
此外,该方法可以通过微分脉冲伏安法进行优化,用以对抗坏血酸干扰下的多巴胺进行检测,并显示出可用的分析参数,即:一个0–130 uM的线性范围,一个(6.318 ± 0.002) uA mM-1的灵敏度,一个(11 ± 0.1) uM的检测极限和一个(37 ± 0.2) uM的量化极限,这些参数使商业制药的规模生产成为可能。
关键词:多巴胺抗坏血酸 CTAB(十六烷基三甲基溴化铵)Title:Influence of CTAB on the electrochemical behavior of dopamine and ascorbic acidAbstract:This research work concerns the electrochemical study of dopamine and ascorbic acid in the presence of the cationic surfactant cetyltrimethylammonium bromide.From this study is possible to note that the cetyltrimethylammonium bromide greatest influence was on the dopamine, because it disfavors both its oxidation and reduction, thereby giving a smaller heterogeneous rate constant, k0, value than in its absence, provoking that the process tends to irreversibility. On the contrary, for the ascorbic acid case, its oxidation was favored.These effects can influence the separation of the dopamine and ascorbic acid voltammetric signals up to 453 mV. Further, the method could be optimized through differential pulse voltammetry to proceed with the analytic determination of dopamine in the presence of ascorbic acid displaying usable analytic parameters, namely: a linearity range of 0–130 lM, a sensitivity of (6.318 ± 0.002) lA mM-1, a detection limit of (11 ± 0.1) lM, and a quantification limit of (37 ± 0.2) lM, which made it possible to effect the quantification on a commercial pharmaceutical sample.Keywords:Dopamine Ascorbic acid CTAB目录中文摘要 (I)Abstract: (II)第一章文献综述................................................... - 1 -1.1 电化学分析方法简介.......................................... - 1 -1.1.1 电分析化学的发展 ...................................... - 1 -1.1.2 电分析化学的特征 ...................................... - 3 -1.1.3 电分析化学的分类[17] .................................... - 3 -1.2 表面活性剂.................................................. - 4 -1.2.1 阳离子表面活性剂简介 .................................. - 5 -1.2.2 表面活性剂的临界胶束浓度[22-24]........................... - 5 -1.2.3 表面活性剂在电分析中的应用[27] .......................... - 6 -1.2.4 表面活性剂的作用[28] .................................... - 6 -1.3 多巴胺及抗坏血酸简介和用途.................................. - 7 -1.3.1 多巴胺及其用途[29-31]..................................... - 7 -1.3.2抗坏血酸及其用途[32-34] ................................... - 8 -1.4 立题依据、研究内容和创新性.................................. - 9 -1.4.1 立题依据 .............................................. - 9 -1.4.2 研究内容 ............................................. - 10 -1.4.3 课题的创新性 ......................................... - 10 - 第二章实验部分 ................................................... - 11 -2.1 试剂及仪器................................................. - 11 -2.1.1 实验试剂 ............................................. - 11 -2.1.2 实验仪器 ............................................. - 12 -2.2 实验装置................................................... - 12 -2.3 实验条件................................................... - 12 -2.3.1 多巴胺及抗坏血酸的浓度 ............................... - 12 -2.3.2 反应温度 ............................................. - 13 -2.4 多巴胺、抗坏血酸和CTAB在玻碳电极上的电化学行为............ - 13 -2.5 CTAB对于多巴胺和抗坏血酸电分析的影响 ...................... - 14 -2.6 CTAB浓度对AA和DA混合后电分析的影响 ...................... - 15 -2.7溶液pH值对AA和DA混合后电分析的影响 ...................... - 15 -2.8多巴胺的线性范围和最低检测限 ............................... - 16 -2.9抗坏血酸的线性范围和最低检测限 ............................. - 18 - 第三章结果与讨论 ................................................. - 19 -3.1 抗坏血酸、多巴胺和 CTAB在玻碳电极上的电化学行为 ........... - 19 -3.2 CTAB对于多巴胺和抗坏血酸电分析的影响 ...................... - 22 -3.3 CTAB浓度对AA和DA混合后电分析的影响 ...................... - 28 -3.4 溶液pH值对抗坏血酸和多巴胺混合后电分析的影响.............. - 31 -3.5 多巴胺的线性范围和最低检测限............................... - 32 -3.6 抗坏血酸的线性范围和最低检测限............................. - 33 -第四章结论 ....................................................... - 35 -4.1 实验结论................................................... - 35 -4.2 实验总结................................................... - 35 - 参考文献 .......................................................... - 36 - 致谢 .......................................................... - 38 -第一章文献综述电分析化学是仪器分析化学的一个重要的分支,它是以测量某一化学体系或者试剂的电反应为基础建立起来的一类化学分析方法。
化妆品原料中盐含量的要求
化妆品原料中盐含量的要求英文回答:The requirement for salt content in cosmetic ingredients varies depending on the specific product andits intended use. In general, the salt content in cosmetics should be kept at a low level to prevent any potential skin irritation or drying effects. However, certain products, such as bath salts or exfoliating scrubs, may contain higher levels of salt for their specific purposes.For example, let's consider a facial cleanser. A good facial cleanser should have a balanced pH level and should not contain excessive salt. High salt content can strip the skin of its natural oils and cause dryness. Therefore, itis important to choose a facial cleanser with a low salt content to maintain the skin's moisture balance.On the other hand, bath salts are specifically designed to be added to bathwater for relaxation and therapeuticpurposes. These products often contain a higher salt content, as the salt helps to soften the water and providea soothing effect on the skin. However, it is still important to use bath salts in moderation and follow the recommended usage instructions to avoid any adverse effects.In addition to the specific product requirements, regulatory bodies such as the Food and Drug Administration (FDA) in the United States also impose certain limits onthe salt content in cosmetics. These regulations are in place to ensure consumer safety and prevent any potential harm from excessive salt exposure.中文回答:化妆品原料中盐的含量要求因具体产品及其预期使用目的而异。
DIBAL-H选择还原酯基而不影响苄溴
1250J.Med.Chem.2010,53,1250–1260DOI:10.1021/jm901530bSynthesis and Structure-Activity Relationships of Azamacrocyclic C-X-C Chemokine Receptor4 Antagonists:Analogues Containing a Single Azamacrocyclic Ring are Potent Inhibitors of T-Cell Tropic(X4)HIV-1ReplicationGary J.Bridger,*,†Renato T.Skerlj,†,)Pedro E.Hernandez-Abad,‡David E.Bogucki,†Zhongren Wang,†Yuanxi Zhou,†Susan Nan,†Eva M.Boehringer,†Trevor Wilson,†Jason Crawford,†Markus Metz,†,)Sigrid Hatse,§Katrien Princen,§Erik De Clercq,§and Dominique Schols§†AnorMED Inc.now Genzyme Corporation,500Kendall Street,Cambridge,Massachusetts02142,‡Johnson Matthey Pharmaceutical Research,1401King Road,West Chester,Pennsylvania19380,and§Rega Institute for Medical Research,Katholieke Universiteit Leuven, Minderbroedersstraat10,B-3000Leuven,Belgium.)Genzyme Corp.,153Second Avenue,Waltham,Massachusetts02451.Received October15,2009Bis-tetraazamacrocycles such as the bicyclam AMD3100(1)are a class of potent and selective anti-HIV-1agents that inhibit virus replication by binding to the chemokine receptor CXCR4,the coreceptor for entryof X4viruses.By sequential replacement and/or deletion of the amino groups within the azamacrocyclic ringsystems,we have determined the minimum structural features required for potent antiviral activity in thisclass of compounds.All eight amino groups are not required for activity,the critical amino groups on a perring basis are nonidentical,and the overall charge at physiological pH can be reduced without compromisingpotency.This approach led to the identification of several single ring azamacrocyclic analogues such asAMD3465(3d),36,and40,which exhibit EC50’s against the cytopathic effects of HIV-1of9.0,1.0,and4.0nM,respectively,antiviral potencies that are comparable to1(EC50against HIV-1of4.0nM).Moreimportantly,however,the key structural elements of1required for antiviral activity may facilitate the designof nonmacrocyclic CXCR4antagonists suitable for HIV treatment via oral administration.IntroductionThe development of antiviral agents that inhibit alternative targets in the HIV a-replicative cycle remains an important goal in order to alleviate the side effects of currently approved agents or to overcome the problem of drug resistance.In this regard,we have focused on the development of compounds that inhibit CXCR4,the coreceptor used by T-tropic(T-cell tropic)viruses for fusion and entry of HIV into target cells of the immune system.The corresponding chemokine receptor CCR5is used by M-tropic(macrophage tropic)viruses and has been associated with the early stages of infection and replication in HIV-positive patients.1,2The transition from M-tropic to T-tropic(or dual/mixed-tropic)virus during the course of HIV infection in approximately50%of patients is associated with a faster CD4þT-cell decline and a more rapid disease progression.3-5Recently,we reported the results of clinical trials with our prototype CXCR4antagonist AMD31006-8(1)and an orally bioavailable CXCR4antagonist,(S)-N0-(1H-benzimidazol-2-ylmethyl)-N0-(5,6,7,8-tetrahydroquinolin-8-yl)butane-1,4-dia-mine(AMD070).9-11When administered to HIV positive patients whose virus was confirmed to use CXCR4for viral entry,both agents were able to suppress the replication of CXCR4and dual-tropic strains of HIV.Similarly,the CCR5 antagonist Maraviroc suppresses replication of HIV-1that exclusively uses CCR5for entry12and was recently approved by the FDA for combined antiretroviral therapy in treatment-experienced patients.13A combination of CCR5and CXCR4 antagonists for treatment of dual/mixed-tropic HIV infection is therefore highly desirable.Beyond its use as a coreceptor for HIV,the CXCR4 chemokine receptor has a more fundamental role in the trafficking of white blood cells,which broadly express CXCR4.14,15A member of the superfamily of G-protein coupled receptors,the interaction of CXCR4and its ligand, stromal cell-derived factor-1(SDF-1),plays a central role in the homing and retention of cells within the bone marrow microenvironment.16Consistent with these observations,ad-ministration of1to healthy volunteers caused a dose-depen-dent leukocytosis6,7that in subsequent studies was shown to include the mobilization of CD34þstem and progenitor cells suitable for hematopoietic stem cell transplantation.17-20The ability of analogues of1to mobilize progenitors correlated with their in vitro capacity to inhibit SDF-1binding to CXCR4.21Because of the need for parenteral administration, 1was developed in combination with granulocyte colony-stimulating factor(G-CSF)to mobilize hematopoietic stem cells to the peripheral blood for collection and subsequent autologous transplantation in patients with non-Hodgkin’s lymphoma(NHL)and multiple myeloma(MM).22-25Plerix-afor(1)was approved by the FDA in December2008.We have previously reported the structure-activity rela-tionships of anti-HIV bis-azamacrocycles and their transition*To whom correspondence should be addressed.Phone:617-429-7994.Fax:617-768-9809.E-mail:gary.bridger@.Ad-dress:Gary J.Bridger,Genzyme Corporation,55Cambridge Parkway,Cambridge MA02142.a Abbreviations:HIV,Human Immunodeficiency Virus;CXCR4,C-X-C chemokine receptor4;CCR5,C-C-R chemokine receptor5./jmc Published on Web12/31/2009r2009American Chemical SocietyArticle Journal of Medicinal Chemistry,2010,Vol.53,No.31251 metal complexes in detail.26-28Because of the commonstructural features between a doubly protonated cyclam(1,4,8,11-tetraazacyclotetradecane)ring present in1(at phy-siological pH)and a kinetically labile transition metal com-plex of cyclam with an overall charge ofþ2,we proposed thatboth structural motifs may bind to the CXCR4receptorthrough interactions with amino acid residues containingcarboxylate groups.29We have subsequently shown via direc-ted mutagenesis of the aspartate and glutamic acid residues inCXCR4that binding of1and related analogues to the seventransmembrane,G-protein coupled receptor is highly depen-dent upon the amino acids Asp171and Asp262,located intransmembrane region(TM)-IV and TM-VI at each end ofthe main ligand binding crevice of the receptor.30-35Mutationof either aspartic acid to aspargine significantly reduced theability of1to inhibit binding of radiolabeled stromal cellderived factor-1R(125I-Met-SDF-1R).More importantly,however,U87cells stably transfected with CD4and themutant coreceptors CXCR4[D171N]and CXCR4[D262N]were less effective at supporting infection of the CXCR4-usingHIV-1strain NL4.3compared to the wild-type receptor andthe double mutant CXCR4[D171N,D262N]completely failedas a coreceptor for HIV infection.31Correspondingly,theability of1to inhibit HIV-1infection via CXCR4[D171N]andCXCR4[D262N]was also diminished,thereby confirmingthat1binds in a region of the receptor that is critical for X4HIV-1coreceptor function.We have also reported that binding of the bis-Zn,Ni,andCu complexes of1were also dependent upon D171and D262of the receptor.36In a similar manner to1,the transitionmetal complexes were found to be less effective inhibitors of125I-Met-SDF-1R binding to the mutant receptors CXCR4-[D171N]and CXCR4[D262N]compared to the wild-typereceptor.Incorporation of Zn,Ni,or Cu into the cyclam ringsof1increased the affinity to the wild-type CXCR4receptor,but the enhancement was selectively eliminated by substitu-tion of Asp262.Supporting physiochemical evidence for theinteraction of acetate(carboxylates)with metal complexes ofazamacrocycles,including1,has been recently reported.37,38In the current study,we determine the minimum struc-tural features of1required for potent antiviral activity, leading to the identification of the single azamacrocyclic ring analogue AMD346532,33,39,40(3d)and ultimately the design of nonmacrocyclic,orally biovailable CXCR4an-tagonists.11,41,42Given the growing body of evidence that the CXCR4/SDF-1interaction is involved in regulating several human malignancies,43-45CXCR4antagonists may have additional therapeutic applications in addition to HIV treatment.ChemistryAnalogues containing a single1,4,8,11-tetraazacyclotetra-decane(cyclam)ring were prepared by modifications to previously published routes26,29as shown in Scheme1.Reac-tion of the selectively protected tris-diethylphosphoramidate (Dep)cyclam ring(2a)with R,R-dibromo-p-xylene in aceto-nitrile containing potassium carbonate gave the desired bro-momethyl intermediate(2b).Reaction of the bromide with an excess of the requisite amine,followed by deprotection of the Dep-groups with a saturated solution of hydrogen bromide in acetic acid at room temperature.gave analogues3a-i as the corresponding hydrobromide salts.To prepare analogues of3d in which the cyclam ring was replaced by a series of14-membered azamacrocyclic rings,we prepared a series of selectively protected macrocyclic ring systems containing a single(unprotected)secondary amine. This approach ensures the regiochemical outcome of the reaction with a benzylic halide during final construction (as shown in Scheme6).The syntheses of appropriate pre-cursors are shown in Schemes2-5.To incorporate fluorine groups at the desired position in the macrocyclic ring,suitably fluorinated bis-electrophiles were prepared,starting from 4-oxo-heptanedioic acid diethyl ester(4)and heptane-1,4,7-triol(8)as depicted in Scheme2.Reaction of the ketone(4) with neat(diethylamino)-sulfur trifluoride46,47(DAST)at room temperature for12days gave the corresponding di-fluoro-intermediate(5)in43%yield.Reduction of the ester groups with LAH(to give the diol6),followed by derivatiza-tion with toluenesulfonyl chloride,gave the bis-electrophile (7)required for the impending macrocyclization reaction.The corresponding monofluorinated intermediate was prepared in a similar manner.Protection of the primary alcohols in8as the acetyl group using acetic anhydride gave the secondary alcohol9,which was rapidly(and virtually quantitatively) converted to the fluorinated intermediate(10)with DAST (2.0equiv)in dichloromethane.Removal of the acetyl pro-tecting groups with saturated ammonia in methanol,followed by reaction of the diol(11)with p-toluenesulfonyl chloride, Scheme1aa Reagents:(a)R,R0-dibromo-p-xylene,K2CO3,CH3CN,reflux;(b)amine,K2CO3,CH3CN,reflux;(c)HBr,acetic acid,room temp. Scheme2aa Reagents:(a)Et2NSF3(neat),room temp;(b)LAH,Et2O;(c)Ts-Cl,Et3N,CH2Cl2;(d)acetic anhydride,pyridine;(e)Et2NSF3, CH2Cl2,-78°C,then room temp;(f)NH3/MeOH,room temp;(g)Ts-Cl,Et3N,CH2Cl2.1252Journal of Medicinal Chemistry,2010,Vol.53,No.3Bridger et al.gave the desired bis-electrophile 12containing a single fluorine group.The selectively protected azamacrocyclic rings were pre-pared via directed combinatorial macrocyclization of bis-2-nitrobenzenesulfonamides 48(Ns)(15a -c ,16a -c ,18)with bis-electrophiles (7,12,17)using previously optimized condi-tions 28(Scheme 3).To incorporate a phenyl or heterocyclic ring into the macrocycle,the corresponding bis-2-nitrobenze-nesulfonamide (15a -c )was prepared from the bis-aminoethyl intermediates 28(13a -c )by reaction with nosyl chloride (Et 3N,CH 2Cl 2).Similarly,16a ,b were obtained by reac-tion of commercially available intermediates 14a ,b with nosyl chloride or in the case of 16c (X=S)by reduction of 3,30-thiodipropionitrile with BH 33Me 2S and reaction of the intermediate diamine (14c )with nosyl chloride to give 16c .Macrocyclization was accomplished by dropwise addition of a DMF solution of the bis-electrophile to a DMF solution of the bis-2-nitrobenzenesulfonamide containing Cs 2CO 3maintained at a temperature of 80°C.Standard workup,followed by purification of the crude product by column chromatography on silica gel,gave the desired macrocycles 19a -c ,20a -c ,and 21a ,b in yields of 19-55%.Reaction of theintermediates from above with HBr/acetic acid at room temperature gave 22a -c ,23a -c ,and 24a ,b ,respectively.Because of synthetic convenience,we also prepared the selectively protected “isomers”of 22a ,b and 23a in which the alternative secondary amine was available for the alkylation reaction.We reasoned that reaction of 19a ,b and 20a with approximately 1equiv of thiophenol 49(our reagent of choice for nosyl deprotections)may allow pseudoselective deprotec-tion of a single nosyl group,leaving the Dep group intact.After some optimization,we found that reaction of 19a ,b and 20a with 0.8equiv of thiophenol and potassium carbonate in DMF (or acetonitrile)gave the precursors 25and 26a ,b in manageable,albeit modest yields (20-50%)following col-umn purification on silica gel (Scheme 4).Finally,the inter-mediates 27a ,b and 28(Scheme 5)were synthesized as recently described by palladium(0)catalyzed coupling of organozinc iodide reagents with bromopyridines.50Having completed the series of selectively protected aza-macrocycles,we proceeded to completion of the desired analogues by straightforward installation of the right-hand portion containing the aminomethyl pyridine moiety.As shown in Scheme 6,this was accomplished in all cases by direct alkylation of the available secondary amine of the macrocycle with the benzylic chlorides 34a ,b .Intermediate 34a was prepared in four steps from 4-bromomethyl benzoic acid methyl ester (29)and 2-aminomethylpyridine (31):con-version of 31to the 2-nitrobenzenesulfonamide 32,followed by alkylation with the benzyl bromide 30(obtained by reduc-tion of 29with DIBAL-H)gave the desired alcohol 33.As previously reported,28reaction of benzylic alcohols such as 33with methanesulfonyl chloride gave the chloride 34a rather than the corresponding mesylate,presumably via in situ nucleophilic substitution of the initially formed mesylate with chloride.Intermediate 34b (Scheme 6)containing a Dep-protecting group was prepared by an alternative synthesisScheme 3aaReagents:(a)Ns-Cl,Et 3N,CH 2Cl 2;(b)Cs 2CO 3,DMF,80°C;(c)HBr(g),AcOH,room temp.Scheme4Scheme5Article Journal of Medicinal Chemistry,2010,Vol.53,No.31253(procedures in Supporting Information).Alkylation of the available secondary amine of the macrocycles with 34a (or 34b )in CH 3CN in the presence of K 2CO 3gave the penultimate intermediates 35a -n .Deprotection of the nosyl groups with thiophenol and K 2CO 3in DMF gave the free base of the desired analogues,which in the vast majority of cases were converted to the corresponding hydrobromide salts.For analogues derived from the macrocyclic precursors 25and 26a ,b ,the intermediates isolated prior to the deprotection also contained a residual Dep group in addition to nosyl groups.For compound 45,we found that conversion to the hydro-bromide salt using a saturated solution of HBr in acetic acid resulted in concomitant deprotection of the remaining Dep group to obtain compound 45.For compounds 44and 46,the residual Dep group was removed prior to nosyl deprotection and salt formation.The thioether analogue 41a was also used to prepare the corresponding sulfoxide and sulfone analogues for antiviral evaluation as shown in Scheme 7.Initially,we globally protected the amino groups of 41a with Boc and subjected this intermediate to oxidation with oxone in MeOH 51at -10°C to give a mixture of the sulfoxide and sulfone that were separated by column chromatography on silica gel.However,while deprotection of the Boc groups with simulta-neous conversion to the hydrobromide salt proceeded without incident for the sulfone (to give 41c ),we found that deprotec-tion of the corresponding sulfoxide led to substantial reduc-tion and hence recovery of the starting analogue 41a .To overcome this problem,the sulfoxide was synthesized by direct oxidation of 41a with 1equiv of oxone in MeOH to give 41b in a 21%isolated yield and was subsequently tested as the free base in antiviral assays.Finally,we prepared a short series of analogues containing a carbon atom in place of a tertiary nitrogen group at the ring junction.To economize on the number of synthetic steps,weelected to synthesize the dimesylate 54(Scheme 8),an inter-mediate that could be commonly used for the synthesis of multiple analogues via macrocylization with the bis-2-nitro-benzenesulfonamide precursors already in our possession (namely 15a ,16a ,b from Scheme 3).Intermediate 54was prepared from the commercially available starting material bromo-p -tolunitrile via a double one-carbon homologation of the malonate 51,followed by derivatization to gave the requisite bis-methanesulfonate 54.Macrocyclizations of 54with bis-sulfonamides 15a and 16a ,b were performed as described above.Deprotection of the nosyl groups followed by conversion to the corresponding hydrobromide salts gave analogues 56and 58a ,b .DiscussionHaving previously established the optimum ring size and distance between the amines of both aliphatic andScheme 6a aReagents:(a)DIBAL-H,CH 2Cl 2;(b)Ns-Cl,Et 3N,CH 2Cl 2;(c)K 2CO 3,CH 3CN,60°C;(d)Ms-Cl,Et 3N,CH 2Cl 2;(e)K 2CO 3,CH 3CN,80°C;(f)R =Ns:thiophenol,K 2CO 3,DMF,or R =Dep:HBr(g),AcOH,room temp.Scheme 7aaReagents:(a)oxone,MeOH,-10°C;(b)(Boc)2O,THF;(c)HBr(g),AcOH,room temp.Scheme 8aaReagents:(a)NaH,R -bromo-tolunitrile,THF;(b)LiAlH 4,THF;(c)Ns-Cl,Et 3N,CH 2Cl 2;(d)2-picolyl chloride,Et 3N,K 2CO 3,KBr,CH 3CN,reflux;(e)Ms-Cl,Et 3N,CH 2Cl 2;(f)cetyltrimethyammonium bromide,NaCN,benzene,H 2O,reflux;(g)conc HCl/AcOH (4:1),reflux;(h)BH 3.Me 2S,THF;(i)Ms-Cl,Et 3N,CH 2Cl 2;(j)Cs 2CO 3,DMF,80°C;(k)thiophenol,K 2CO 3,CH 3CN (or DMF),40°C.1254Journal of Medicinal Chemistry,2010,Vol.53,No.3Bridger et al.pyridine-fused bis-tetraazamacrocycles required for potent X4anti-HIV activity,we designed a series of compounds to address the question of structural redundancy.The prototype bis-macrocycle 1has a center of symmetry and contains eight amino groups,of which four are positively charged at phy-siological pH.In the current study,we aimed to answer two specific questions:(1)Are all four positive charges required for potent anti-HIV activity?(2)On a per ring basis,what are the minimum structural requirements for activity?Assuming that the structural requirements are not iden-tical for both rings of 1,we reasoned that the simplest replacement for a single tetraaza-macrocyclic ring would be a pseudo diamine-segment,representing the first two amino groups of the macrocyclic ring from the point of attachment at the benzylic position.A judicious choice of “diamine”would also reduce the overall charge to þ1.Having previously established that the optimum distance between the first two amino groups was a two-carbon unit,we prepared a series of aminomethyl-substituted analogues in which the second amino group was a substituent upon an aromatic ring or part of a heterocyclic ring.In either case,the second p K a would be sufficiently low to prevent a second protonation at physiological pH.The compounds were tested for their ability to inhibit replication of HIV-1III B in MT-4cells,a strain of HIV-1that uses exclusively CXCR4for fusion and viral entry into target cells.The results are shown in Table 1.Compared to 1,the introduction of a benzylamine group (3a )in place of the azamacrocyclic ring substantially reduced anti-HIV potency,although the compound remained active at submicromolar concentrations.The concentration of 3a re-quired to inhibit HIV-1replication by 50%(the EC 50)was 0.49μM,which was approximately 100-fold higher than the 50%inhibitory concentration of 1.Aromatic amino groups at the 2-position (3b )or 4-position (3c )did not affect antiviral potency.Both 3b ,c exhibited comparable EC 50’s to the un-substituted benzyl group (3a ).However,we observed a sub-stantial increase in anti-HIV potency when the benzyl group was replaced by a pyridyl group (3d ).Compound 3d exhibited a 50%inhibitory concentration of 0.009μM,which was only ca.2-fold higher than the EC 50of 1.Furthermore,the 50%cytotoxic concentration (CC 50)of compound 3d in MT-4cells was greater than 112μM.Thus 3d exhibits a selectivity index of greater than 12000.The positional specificity of the pyridine-N in 3d was also examined.Replacement of the 2-pyridyl group with the 3-pyridyl (3e )or 4-pyridyl (3f )group had a detrimental effect on anti-HIV potency.For example,the EC 50’s of analogues 3e ,f were approximately 3orders of magnitude higher than the concentration of 3d required to inhibit HIV-1replication by 50%(the EC 50’s of 3e and 3f were 8.470and 9.977μM,respectively).Methylation of the amine in 3d (to give 3g )or extension of the connectivity to an aminoethyl pyridine group (to give 3h )also adversely affected the anti-HIV potency.Finally,we replaced the pyridine moiety with a comparable heterocycle of lower p K a than pyridine,namely the pyrazine group (3i ).Perhaps not surprisingly,the antiviral potency of analogue 3i was approximately comparable to the benzyl analogue 3a ,which did not contain a vicinal heterocycle nitrogen atom.With the optimized “right-hand”replacement for the aza-macrocycle ring of 1fixed as the 2-aminomethyl pyridine group,we then turned our attention to the “left-hand”ring.Needless to say,the mandatory synthesis of the symmetrical analogue in which both rings were replaced by a 2-amino-methyl pyridine group turned out to be a predictably fruitless exercise (EC 50was >250μM,data not shown).We therefore focused on systematically replacing individual amine groups of the left ring.As shown in Table 2,we first prepared an analogue in which the [14]aneN 4(cyclam)ring had been replaced by the optimized and equally suitable,py[iso -14]-aneN 4ring (to give compound 36).Consistent with the structure -activity relationship of py[iso -14]aneN 4bis-azama-crocycles,compound 36proved to be a potent inhibitor of HIV-1replication,exhibiting an EC 50of 0.001μM,that is,around 9-fold and 4-fold lower,respectively,than the con-centration of 3d or 1required to inhibit viral replication by 50%.Although the pyridine-N of the macrocyclic ring in 36was previously found to be critical for high antiviral potency,we reasoned that a precise determination of the pyridine-N contribution to potency could help redesign a less basic pounds 37and 38were then prepared to answer this question.Both analogues 37,containing a phenyl replacement and 38,containing an “exocyclic”pyridine fused group,retained reasonable anti-HIV potency (the EC 50’s of 37and 38were 0.040and 0.104μM,respectively)but were at least 40-to 100-fold less potent than analogue 36.So what role does the pyridine group play?At physiological pH,the overall charge of the py[iso -14]-aneN 4ring in 36is also þ2(in a similar manner to cyclam 52)and the likely protonation sequence is indicated in Figure 1A,based on the sequence reported by Delgado et al.53for similar 14-membered tetraazamacrocyclic rings contain-ing pyridine.Presumably,the secondary amino groups are predominantly protonated and the overall structure is stabi-lized by intramolecular hydrogen bond interactions from the adjacent hydrogen-bond acceptors,the pyridine and tertiary benzylic amine groups (while minimizing the elec-trostatic repulsion of two positive charges in a confined macrocyclic ring).This is confirmed by a conformational analysis of 36on B3LYP/6-31G*level followed by single point energy calculations.In the energetically most stable ring conformation (LMP2/6-311þG*þZPE),the pyridine nitro-gen forms two six-membered intramolecular hydrogen bond interactions with the two adjacent protonated nitrogens as shown in Figure 2.Potential five-membered intramolecular hydrogen bond interactions are formed with the tertiary amine.Table 1.Antiviral Activity of Single RingAzamacrocyclesnR 1R 2HIV-1(III B )EC 50(μM)MT-4cells CC 50(μM)3a 1H Ph0.4911603b 1H 2-amino-Ph 1.825243c 1H 4-amino-Ph 0.7172273d 1H 2-pyridine 0.009>1123e 1H 3-pyridine 8.470373f 1H 4-pyridine 9.977>2793g 1Me 2-pyridine 0.416383h 2H 2-pyridine 49.135>1103I 1H5-Me-pyrazine1.8957810.004>421ArticleJournal of Medicinal Chemistry,2010,Vol.53,No.31255The stabilization provided by this “shared”protonated structure could account for the high basicity of azamacrocyc-lic rings,as suggested by Kimura et al.54It did not seem unreasonable,therefore,that a potential role of the pyridine group is the contribution of a single intramolecular hydrogen-bond,which locks the conformation of the protonated aza-macrocyclic ring in manner that is beneficial to antiviral potency.To test this hypothesis,we prepared a series of analogues (depicted in Figure 1B,data in Table 2)in which the fused aromatic group had been removed and replaced by an aliphatic group,in some cases containing a hydrogen-bondacceptor at the key position “x,”the position occupied by the pyridine nitrogen in compound 36.Consistent with the hydrogen-bonding hypothesis,the alkyl analogue 39exhibited an anti-HIV potency that was compar-able to the phenyl and exocyclic pyridine analogues 37and 38(the EC 50’s of 37and 39,were 0.040and 0.043μM,re-spectively).This result categorically rules out the possibility that the conformational restrictions imposed by the fused aromatic groups in compounds 37,38were even partially responsible for the high potency of 36.However,incorpora-tion of a hydrogen-bond acceptor at position x (Figure 1B)in some cases restored activity comparable to 36.For example,the oxygen analogue 40exhibited an EC 50that was only 4-fold higher than the concentration of 36required to inhibit HIV-1replication by 50%(the EC 50of 40was 0.004μM).The corresponding thioether analogue 41a exhibited an EC 50of 0.013μM,which is approximately 3-fold higher than com-pound 40.Although the antiviral potency of the thioether analogue 41a compared to the ether analogue 41is greater than one would predict from the strength of the hydrogen-bond acceptor acceptor capabilities (thioether groups are considerably weaker H-bond acceptors than the oxygen inTable 2.Antiviral Activity of Single RingAzamacrocyclesFigure 1.Proposed hydrogen-bond structure of protonated aza-macrocycles.1256Journal of Medicinal Chemistry,2010,Vol.53,No.3Bridger et al.40),this result can be reconciled by considering the nature of the H-bond required;a six-membered intramolecular H-bond constrained by the macrocyclic ring (Figure 2).With the thioether compound 41a in hand,we also pre-pared the sulfoxide (41b )and sulfone (41c )analogues by direct oxidation of 41a .We reasoned that the oxygen atoms of the sulfoxide and sulfone are stronger H-bond acceptors than the sulfur atom of 41a and may consequently improve the anti-HIV potency.However,both 41b and 41c were considerably weaker antiviral agents,exhibiting 50%effective concentra-tions for inhibition of HIV-1replication that were at least 79-fold higher than the EC 50of 41a (the EC 50’s of 41b and 41c were 0.485and 11.878μM,respectively).The precise reason for the poor antiviral activity exhibited by analogues 41b ,c was unclear;although the sulfoxide and sulfone are more sterically demanding than the thioether and could induce a ring conformation that is detrimental to antiviral activity,we could not rule out the possibility that the H-bond acceptor oxygen is now “one-bond”outside of the ring,and the intramolecular H-bond itself induces an unfavorable confor-mation (a seven-membered ring H-bond in 41b ,c (Figure 2)compared to a six-membered in 41a ).To complete this series of compounds therefore,we decided to introduce the fluoro and difluoro substituents at position x (Figure 1B).Several reports have demonstrated that the fluoro group can partici-pate as an acceptor for intramolecular H-bonds,particularly within highly constrained ring structures.55-57This is also confirmed by our calculations,as shown in Figure 2.The fluoro (43)and difluoro (42)analogues were also attractive substituents for two other reasons:(1)the substituents would be situated at the fourth carbon from the adjacent amine group,thereby minimizing the affect on p K a ;(2)in a similar manner to the sulfoxide and sulfone,the H-bond acceptor would be one-bond outside of the macrocyclic ring.However in this case,because the fluorine atom in C -F groups is isostructural with hydrogen,a negative effect of the fluoro substituents on antiviral activity can only be attributed to an inappropriately positioned H-bond rather than steric requirements (that is,in the absence of an H-bond,we would expect the fluoro or difluoro analogues to exhibit an EC 50comparable to the methylene analogue 39).In antiviral test-ing,the fluoro (43)and difluoro (42)analogues displayed EC 50’s that were greater than 20-fold higher than the methy-lene analogue 39(the EC 50’s of 39,42,and 43were 0.043,0.920,and 1.239μM,respectively),confirming the negative consequences of an incorrectly positioned hydrogen-bond (Figure 2).Next,we focused on the sequence of aliphatic amine groups in the macrocyclic ring required for potent antiviral activity.By straightforward synthetic manipulation of our collection of ring systems,we prepared the structural isomers of analo-gues 36,37,and 39in which the side-chain (R,in Table 2)was connected to the alternative secondary amine group to give compounds 44,45,and 46.In antiviral testing,analogue 44was substantially less potent than its corresponding regioi-somer 39:the EC 50of 44was 11.131μM,which was approxi-mately 260-fold higher than the EC 50of 39.A similar loss of antiviral potency was observed with the phenyl analogue 46and its isomer 37(the EC 50’s of 46and 37were 14.106and 0.040μM,respectively).Interestingly,the loss of antiviral potency with the pyridine-fused isomer 45compared to 36was significant but not as substantial;the EC 50of 45was 0.063μM,around 60-fold higher than the concentration of 36required to inhibit HIV-1replication by 50%.There was a possibility,therefore,that while the “tri-aza”ring configura-tion required for potent antiviral activity is clearlyrepresentedFigure 2.Lowest energy conformations of compounds 36,40,41c ,and 42.View from top on a plane defined by three nitrogens and X (see Figure 1).Dashed lines indicate hydrogen bond interactions:the hydrogen bond acceptors in 36and 40are in one plane with the three nitrogens.This is not the case for 41c and 42.Bond angles:36:—(N 333H -N þ)=140.5°,122.4°,102.1°,108.4°.40:—(O 333H -N þ)=135.1°,141.5°;—(N 333H -N þ)=104.6°,102.8°.41c :—(O 333H -N þ)=112.8°,112.8°;—(N 333H -N þ)=108.2°,108.0°.42:—(F 333H -N þ)=142.2°,142.2°;—(N 333H -N þ)=114.7°,114.7°.。
液相色谱测定水稻组织的糖含量英文
液相色谱测定水稻组织的糖含量英文全文共3篇示例,供读者参考篇1Liquid chromatography is a powerful analytical technique used to separate, identify, and quantify compounds in a variety of samples. In agriculture, liquid chromatography is commonly employed to analyze the composition of plant tissues, including the sugar content of rice tissue. In this article, we will explore the application of liquid chromatography in determining the sugar content of rice tissue.Rice is a staple food consumed by a large portion of the world's population. The sugar content of rice tissue can greatly influence its taste, nutritional value, and cooking properties. Therefore, accurately measuring the sugar content of rice tissue is important for quality control and research purposes.Liquid chromatography is well-suited for analyzing sugar compounds because it provides high sensitivity, resolution, and reproducibility. In the analysis of rice tissue, liquid chromatography is typically coupled with a refractive indexdetector or a mass spectrometer for detecting and quantifying sugar compounds.To determine the sugar content of rice tissue using liquid chromatography, the tissue sample is first extracted to obtain the soluble sugars. The extraction process usually involves grinding the tissue sample and mixing it with a solvent such as water or methanol. The resulting extract is then filtered to remove any solid particles before being injected into the liquid chromatography system.Next, the sugar compounds in the extract are separated on a chromatographic column based on their chemical properties. Sugars such as glucose, fructose, sucrose, and maltose can be separated and quantified using different chromatographic methods, such as ion exchange chromatography, size exclusion chromatography, or reverse-phase chromatography.After separation, the sugar compounds are detected by a suitable detector, and their concentrations are calculated based on their peak areas or peak heights. The results are typically expressed as the amount of each sugar compound per gram of rice tissue.In addition to quantifying individual sugar compounds, liquid chromatography can also be used to analyze the totalsugar content of rice tissue. This is done by summing up the concentrations of all sugar compounds detected in the sample.Overall, liquid chromatography is a valuable tool for determining the sugar content of rice tissue. By providing accurate and reliable results, liquid chromatography helps ensure the quality and nutritional value of rice products. In future research, liquid chromatography may also be used to study the effects of genetic, environmental, and processing factors on the sugar content of rice tissue.In conclusion, liquid chromatography is a versatile technique for analyzing the sugar content of rice tissue. Its high sensitivity, resolution, and reproducibility make it an ideal tool for quality control and research in the field of agriculture. By using liquid chromatography, researchers can gain valuable insights into the composition of rice tissue and develop strategies to improve the quality of rice products.篇2Liquid chromatography is a widely used technique in analytical chemistry for separating and quantifying components of a mixture. In the field of agriculture, liquid chromatography has proven to be a valuable tool for analyzing variouscompounds in plant tissues. In this study, we employed liquid chromatography to determine the sugar content in rice tissues.Rice is a staple food for a large portion of the world's population, and its nutritional value is largely dependent on its sugar content. Sugars are essential components of plants as they serve as a source of energy and play a role in various physiological processes. To assess the sugar content in rice tissues, we utilized a liquid chromatography system equipped with a refractive index detector.First, rice tissues were extracted using a solvent to obtain the sugar components. The extracted samples were then injected into the liquid chromatography system for separation. The sugars were separated based on their affinity to the chromatographic column and eluted sequentially. The refractive index detector was used to measure the concentration of sugars in the eluate.Our results showed that rice tissues contained a significant amount of sugars, with sucrose, glucose, and fructose being the predominant sugars detected. The sugar content varied among different parts of the rice plant, with the highest concentration found in the grains. This finding is consistent with the role of sugars as energy reserves in seeds.In conclusion, liquid chromatography is a powerful technique for analyzing the sugar content in rice tissues. By accurately determining the sugar composition, we gain insight into the nutritional quality of rice and can potentially optimize cultivation practices to enhance sugar content. Further research is warranted to investigate the impact of environmental factors on sugar accumulation in rice tissues.篇3Liquid Chromatography Determination of Sugar Content in Rice TissueIntroduction:Rice is one of the most important staple foods in the world, providing a significant portion of the calorie intake for billions of people. The sugar content in rice tissue plays a crucial role in its taste, nutritional value, and cooking properties. Therefore, accurate quantification of sugar content in rice tissue is essential for assessing its quality and nutritional value.Liquid chromatography is a widely used analytical technique for the separation, identification, and quantification of chemical compounds in complex mixtures. In recent years, liquid chromatography has been increasingly utilized for thedetermination of sugar content in plant tissues due to its high sensitivity, selectivity, and reliability.Experimental:In this study, we aimed to develop a liquid chromatography method for the quantification of sugar content in rice tissue. The procedures are as follows:1. Sample Preparation: Rice tissue samples were collected and homogenized using a mortar and pestle. The homogenized tissue was then extracted with a solvent such as methanol to extract sugar compounds.2. Liquid Chromatography Analysis: The extracted samples were injected into a liquid chromatography system equipped with a suitable column for the separation of sugar compounds. A mobile phase consisting of a mixture of solvents was used to elute the compounds from the column.3. Detection and Quantification: Sugar compounds were detected using a UV detector at a specific wavelength. Quantification was achieved by comparing the peak areas of the sugar compounds with those of standard solutions of known concentrations.Results:The liquid chromatography method developed in this study was able to separate and quantify various sugar compounds in rice tissue samples. The method showed good sensitivity, linearity, and reproducibility for the quantification of sugar content in rice tissue.Conclusion:In conclusion, liquid chromatography is a powerful analytical technique for the determination of sugar content in rice tissue. The method developed in this study can provide accurate and reliable quantitative data on sugar content in rice tissue, which is essential for assessing the quality and nutritional value of rice. Further studies can be conducted to optimize the method and apply it to the analysis of sugar content in other plant tissues.。
注射用艾司奥美拉唑钠丁基橡胶塞中抗氧剂BHT及其氧化产物迁移量的测定
图 9 有关物质 10、11 的可能裂解途径 Fig. 9 Possible fragmentation pathway of related substances 10 and 11
药物分析杂志
Chinese Journal of Pharmaceutical Analysis
药 物 分 析 杂 志 Chin J Pharm Anal 2020,40(10)
·1 8 6 1·
图 10 有关物质 12、15 的可能裂解途径 Fig. 10 Possible fragmentation pathway of related substances 12 and 15
5 讨论
子结构特点等,鉴定了 21 种有关物质可能的化学结
有 关 物 质 11:测 得 有 关 物 质 11 的[M+H]+ 离 子的精确质量为 307.154 5,与离子式[C18H19N4O]+ 相应,保留时间为 13.85 min,有 m/z 280.14、121.04、 93.04 的碎片离子,推测为阿帕替尼脱掉 2- 位氨基 上的 4- 亚甲基吡啶结构所得,m/z 280.14 碎片离子 为母离子脱去 -CN 形成,m/z 121.04 碎片离子为脱掉 4-(1- 氰基环戊烷)苯基氨基侧片片段形成,其推测 可能的裂解途径见图 9。
有 关 物 质 15:测 得 有 关 物 质 15 的[M+H]+ 离 子的精确质量为 212.081 4,与离子式[C12H10N3O]+ 相应,保留时间为 15.25 min,有 m/z 184.09、133.04、 105.04、92.05、80.05 的 碎 片 离 子,与 阿 帕 替 尼 相 比 为脱掉 4-(1- 氰基环戊烷)苯基氨基片段形成的 物 质,结 合 分 子 质 量 推 测 为 发 生 分 子 内 亲 核 取 代 反应环合后形成的副产物,m/z 184.09 的碎片离子 为 母 离 子 脱 掉 CO 所 产 生,m/z 133.04 的 碎 片 离 子 为 母 离 子 脱 掉 吡 啶 结 构 所 得,可 能 的 裂 解 途 径 见 图 10。
依达拉奉右莰醇联合丁苯酞对急性缺血性脑卒中患者临床疗效及S100β蛋白水平的影响
依达拉奉右莰醇联合丁苯酞对急性缺血性脑卒中患者临床疗效及S100β蛋白水平的影响王朝娜① 杨雪华① 【摘要】 目的:探讨急性缺血性脑卒中患者采用依达拉奉右莰醇联合丁苯酞治疗对临床效果及S100β蛋白水平的影响。
方法:选取2021年1月—2023年1月济宁市第三人民医院收治的104例急性缺血性脑卒中患者,以随机数字表法分成研究组(n=52)与对照组(n=52),对照组给予丁苯酞治疗,研究组给予依达拉奉右莰醇联合丁苯酞治疗,比较两组临床疗效、神经功能、日常生活能力、S100β蛋白水平及不良反应。
结果:研究组治疗总有效率(94.23%)较对照组(78.85%)更高,差异有统计学意义(P<0.05);治疗后两组Barthel指数评分均提高,美国国立卫生研究院卒中量表(NIHSS)评分均降低,研究组Barthel指数评分较对照组更高,NIHSS评分较对照组更低,差异均有统计学意义(P<0.05);治疗后两组S100β蛋白水平均降低,研究组较对照组更低,差异均有统计学意义(P<0.05);研究组不良反应发生率(7.69%)与对照组(13.46%)比较差异无统计学意义(P>0.05)。
结论:依达拉奉右莰醇联合丁苯酞用于治疗急性缺血性脑卒中,能够提高临床效果,改善神经功能及S100β蛋白水平,促进日常生活能力提升,避免加重机体不良反应。
【关键词】 依达拉奉右莰醇 丁苯酞 急性缺血性脑卒中 神经功能 S100β蛋白 Effect of Edaravone and Dexborneol Combined with Butylphthalein on Clinical Efficacy and S100β Protein Level in Patients with Acute Ischemic Stroke/WANG Chaona, YANG Xuehua. //Medical Innovation of China, 2024, 21(11): 010-013 [Abstract] Objective: To investigate the effect of Edaravone and Dexborneol combined with Butylphthalein on clinical effect and S100β protein level in patients with acute ischemic stroke. Method: A total of 104 patients with acute ischemic stroke admitted to Jining Third People's Hospital from January 2021 to January 2023 were selected and divided into study group (n=52) and control group (n=52) by random number table method. The control group was treated with Butylphthalein, and the study group was treated with Edaravone and Dexborneol combined with Butylphthalein. The clinical efficacy, neurological function, daily living ability, S100β protein level and adverse reactions were compared between the two groups. Result: The total effective rate of the study group (94.23%) was higher than that of the control group (78.85%), the difference was statistically significant (P<0.05). After treatment, the Barthel index scores of both groups were increased, and the national institutes of health stroke scale (NIHSS) scores were decreased, the Barthel index score of the study group was higher than that of the control group, and the NIHSS score was lower than that of the control group, the differences were statistically significant (P<0.05). After treatment, S100β protein levels were decreased in both groups, and the level in the study group was lower than that in the control group, the differences were statistically significant (P<0.05). There was no significant difference in the incidence of adverse reactions between the study group (7.69%) and the control group (13.46%) (P>0.05). Conclusion: Edaravone and Dexborneol combined with Butylphthalein in the treatment of acute ischemic stroke can improve clinical effect, improve nerve function and S100β protein level, promote the improvement of daily living ability, and avoid aggravating adverse reactions. [Key words] Edaravone and Dexborneol Butylphthalide Acute ischemic stroke Neurological function S100β protein First-author's address: Department of Neurology, Jining Third People's Hospital, Jining 272100, China doi:10.3969/j.issn.1674-4985.2024.11.003①济宁市第三人民医院神经内科 山东 济宁 272100通信作者:王朝娜 急性缺血性脑卒中是一种发病率较高的脑血管疾病,其致病因素较多,包括过氧化、脂质沉积等,易引起动脉粥样硬化,造成局部缺氧缺血,导致脑组织坏死性病变[1]。
亲和层析平衡液 英文
亲和层析平衡液英文Affinity Chromatography Binding Buffer.Affinity chromatography is a powerful technique used to purify proteins based on their specific bindinginteractions with a ligand immobilized on a solid support. The binding buffer, also known as the equilibration buffer, plays a crucial role in maintaining the stability and functionality of the protein during the purification process.The composition of the binding buffer is carefully optimized to provide the optimal environment for specific binding of the target protein to the immobilized ligand. Here are some of the key factors to consider when designing an affinity chromatography binding buffer:Buffer pH:The pH of the binding buffer should be adjusted tomatch the optimal pH for the binding interaction between the protein and the ligand. This can be determined experimentally or obtained from the literature. Maintaining the correct pH is essential for preserving the protein's structure and its ability to bind to the ligand.Ionic Strength:The ionic strength of the binding buffer affects the electrostatic interactions between the protein and the ligand. It is important to optimize the ionic strength to promote specific binding while minimizing non-specific interactions. The ionic strength can be adjusted by adding salts such as NaCl or KCl.Detergents:Detergents are often added to the binding buffer to prevent non-specific interactions between the protein and the solid support. Detergents can disrupt hydrophobic interactions and help solubilize the protein. The type and concentration of detergent used should be carefullyselected to minimize interference with the specific binding interaction.Additives:Specific additives may be added to the binding bufferto enhance the binding affinity or stability of the protein. For example, reducing agents such as DTT or TCEP can beused to maintain the protein's disulfide bonds in a reduced state, which may be necessary for binding to the ligand.Buffer Capacity:The binding buffer should have sufficient buffering capacity to maintain the desired pH during the chromatography process. This is particularly important for long chromatography runs or when using buffers with low buffering capacity.General Composition:A typical affinity chromatography binding buffer maycontain the following components:Tris-HCl (20-50 mM)。
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Tran s.Tian jin Univ.2010,16:405-410DOI 10.1007/s 12209-010-1399-xAccept ed d at e:2009-09-29.Supported by National Natural Science Foundation of Chi na (No.50538086),National Key Basic Research and Development Program of China (“973”,N B63),x Y T f S U y N ,6,,D ,f N ,j @Effect of Chloride Content on Bon d BehaviorBetween FRP and Con crete *PAN Jinlong(潘金龙)1,HUANG Y ifa ng (黄毅方)1,X ING Fe ng(邢锋)2(1.Key Laboratory of Concrete &Prestressed Concrete Structures of Ministry of Education of China,College of Civil Engi-neering,Southeast University,Nanjing 210096,China ;2.College of Civil Engineering,Shenzhen Key Laboratory on Durability of Civil Engineering,Shenzhen University,Shenzhen 518060,China)Tianjin University and Springer-Verlag Berlin Heidelberg 2010Ab stract :For reinforced concrete structures located along the seaside,the penetration of chloride ions into concrete may be a threat to the durability of the structures.Experimental investigations were carried out to study the effect of chloride content on the bond behavior between concrete and fiber reinforced polymer (FRP)plates.Direct shear tests were conducted on the FRP strengthened concrete members.Before testing,the specimens were immersed in NaCl solutions with concentrations ranging from 3%—15%for different time (0—120d).Then,the specimens were dried and tested to obtain the initial and ultimate debonding loads,together with strain distributions along the FRP plates of different load values.The correlations between chloride content and debonding parameters are established.Test results show that the debonding parameters are closely related to the immersing time rather than the chloride content of the solution.Keyword s :fiber reinforced polymer (FRP);concrete;chloride content;direct shear test;debonding behaviorWith the increasing need for strengthening and ret-rofitting concrete structures,external bonding of fiber reinforced polymer (FRP)to the tensile side of concrete members has been established as an efficient and effec-tive method to increase both strength and stiffness [1-3].In real applications,many structures may be located at theseaside,and the penetration of chloride ions(Cl -)into concrete from the seawater poses a threat to the durability of the FRP strengthened concrete structures.Many stud-ies have been performed to investigate the effect of steel corrosion on the strength and mechanical behavior of reinforced concrete (RC)members.It is found that lower degrees of corrosion,ranging from 0to 4%mass loss of steel bars,result in an increase in bond strength between the steel and concrete in the structures,while higher de-grees of corrosion,above 4%mass loss,lead to cracks and rapid decrease in bond strength [4-6].Fortunately,for the concrete structures strengthened by FRP composites,the bonding of FRP plates to the concrete member can stop or slow down the penetrationof Cl -into concrete from the tensile surface.For exam-ple,for the strengthened concrete beams,the bridgingforce in the bonded FRP plates can limit the opening of cracks and play an important role in improving the dura-bility of the strengthened concrete members [7-9].For a carbon fiber reinforced polymer(CFRP)wrapped con-crete beam,CFRP wraps can reduce the steel mass loss as well as the corresponding current [10].One test result shows that the CFRP wrapped RC beams,with 4.6%mass loss of steel,achieve a higher bond stress compared with the uncorroded beams [11].Another experiment indi-cates that the ultimate monotonic strength of the CFRP strengthened corroded RC beams increases to a level be-tween 37%and 87%above the predicted strength of simi-lar unstrengthened uncorroded beams [12].However,forthe unwrapped concrete members,Cl -can still diffuse to the steel surface from the side surfaces or cracked part of the concrete member [13].For the FRP strengthened con-crete members,the bond behavior between FRP and con-crete should be an important issue deserving to be fo-cused on.Based on experimental results,Yang et a l [14]summed up that the bond capacity of FRP-to-concrete interface decreased with the immersing time in the sea-Program o.2009C 2200and the E cellent oung eachers Program o outheast niversit .PA Jinlong born in 197male r associate Pro .Correspondence to PA Jinlong E-mail:i nlongp .Transactions of Tianjin University V ol.16No.62010—6—water,but the bond capacity had little correlation with the concrete compressive strength.Soudki et al [15]reported the results of 11RC beams strengthened with CFRP sheets and subjected to a severe environment (300wet-ting -drying cycles with 3%NaCl ),and found that the ultimate capacity of the CFRP strengthened beams de-creased by 11%—28%,but the stiffness and yield load of the RC beams were not affected by the environmental exposure [15].For the strengthened concrete structures,the durability of adhesive and CFRP composites should also be important problems for their durability.It is found that the extensibility of CFRP plates decreased a little but Young ’s modulus or tensile strength can hardly be af-fected by corrosive environments,such as high and low temperatures,freeze -thaw cycles,dry -humidity cycles [16].Epoxy resin is often used as adhesive for structural strengthening,and its compressive strength decreases with the immersing time in alkaline solution and natural water [17].In this paper,the direct shear test was conducted to investigate the correlation between FRP/concrete bond behavior and chloride content.1Experimental1.1Material propertie sIn this experiment,two batches of concrete prisms were cast for the direct shear tests,and the mixing pro-portions of the components were 1∶0.5∶1.5∶2(ratio of cement to water to sand to aggregate,C ∶W ∶S ∶A in short )and 1∶0.6∶1.5∶2by weight respectively.As for the dimensions,the specimens were 150mm in height,150mm in width,and 550mm in length.Some other concrete cubes were cast to test the compressive strength of concrete for the beam specimens.The elastic modulus of concrete (E C )is listed in Tab.1.Tab.1Material properties of concreteMixing proportion (C ∶W ∶S ∶A)Compressive strength/MPaYoung ’s modulus/GPaBatch 11∶0.5∶1.5∶217.2523.7Batch 21∶0.6∶1.5∶216.0622.9The FRP composites employed in the tests are the carbon fibers from HT300,Nippon Oil Corporation,Ja-pan.The Young ’s modulus of the FRP was tested to be 234GPa and the thickness was 0.165mm per ply accord-ing to the production specifications.The tensile modulus of the epoxy -based adhesive (TATSUHI Co.,Ltd.)used G 1.2Pre pa ration of spe cime nsFourteen specimens were tested for investigating the effect of chloride content on the bond behavior between FRP and concrete.Before applying the FRP composites,the surfaces of concrete prisms were roughened to expose the aggregate for increasing the bond between FRP and concrete.Epoxy resin,with resin/hardener ratio of 2to 1by weight,was used as both matrix for the FRP layers and adhesive between FRP and concrete.In succession,two layers of FRP sheets were bonded to the concrete prisms layer by layer by using the epoxy resin.The con-figuration and geometric dimensions of the prism speci-mens are shown in Fig.1.Four solutions with different concentrations of sodium chloride (NaCl )(3%,6%,10%,and 15%)were applied to the tests,which were much higher in concentration than NaCl in seawater (approxi-mately 2.72%),to speed up the test procedure.The con-crete prisms were entirely immerged into the solutions to ensure that the interface between FRP and concrete could be eroded.After certain days (0d,15d,30d,60d,90d and 120d ),as listed in Tab.2,the concrete prisms were taken out and totally dried for testing.For convenience of description,the notation of the specimens is described as follows.For example,B1-30-10,the first part “B1”de-notes that the specimen was cast with concrete of Batch 1,the second number “30”denotes that the specimen was immersed in the solution for 30d,and the last number “10”denotes that the specimen was immersed in a solu-tion with the Cl -concentration of10%.Fig.1Specimen dimensions1.3T e st setup a nd procedureBefore testing,the specimen should be carefully aligned to make sure that the pulling force is along the vertical plane of the FRP plate so as to reduce any possi-ble peeling effect (Fig.2).The test was conducted under f 540in the tests was tested to be 2.49Pa.displacement control with a loading rate o 0.0mm/min.PAN Jinlong et al:Effect of Chloride Content on Bond Behavior Between FRP and Concrete——Tab.2Environmental exposure situation of all specimensNaCl concentration15d30d60d90d120d0d3%B1-90-3,B2-90-36%B1-90-6,B2-90-610%B1-15-10*B1-30-10*,B1-30-10B1-60-10B1-90-10,B2-90-10B1-120-1015%B1-90-15,B2-90-15B1-0-0*Note:*represen ts that the direct shear test of specimens was conducted on the 120th day,while others on the 380th day.The load value from the material testing system (MTS )was automatically collected.To record the strain varia-tions along the FRP plate during the loading process,eight strain gauges were attached to the FRP plate with a center -to -center spacing of 30mm (Fig.2).Finally,the bonded strain gauges were connected to an automatic data logger (TDS303)to collect the strains during the loadingprocess.Fig.2Test setup2T est results and discussion2.1Fa ilure cha racterizationIn the experiments,the debonding failure of FRP plate was observed for all specimens.With an unbonded zone of 50mm at the pulled end of the FRP plate,wedge failure of concrete was avoided.With increasing external load,debonding started to occur from the loaded end of the FRP plate.After final failure,the FRP plate was en-tirely separated from the concrete prism with a thin layer of concrete attached to its surface.The initial and ulti-mate debonding loads of each specimen were recorded.To illustrate the debonding behavior during the test,the specimen B1-60-10was used as an example.The typical curve of load v ersus global displacement is shown in Fig.3,as well as the curve of load versus relative slip be-tween FRP and concrete collected from linear variable differential transformer (LVDT).The specimen B1-60-10was immersed for 60d in a solution with the chloride concentration of 10%.Before initial debonding (the mo-F 3),x increases linearly with the global displacement of the bonded FRP plate.At this stage,there are no cracks along the concrete/FRP interface and the stresses are transferred from the FRP plate to the concrete prism by the shear deformation of the adhesive layer.After the external load reaches around 13.7kN (the dashed line in Fig.3),initial debonding occurs at the concrete/FRP interface near the pulled end.Then,the external load continues to increase with the debonded zone due to the presence of interfacial friction and interlocking between the failure surfaces.At this stage,the external load increases with the global dis-placement with a smaller slope.The size of the debonded zone grows steadily with the increase of the external load until the load reaches 15.59kN.After that,the global displacement increases significantly,but the external load shows a sudden drop due to the occurrence of unstable debonding,indicating that the ultimate stage is reached.Similar observations are also obtained for other speci-mens during the loadingprocess.Fig.3Load versus global displacement curve for specimen B1-60-10Fig.4shows strain distributions along the FRP plates for specimen B1-60-10.Each curve corresponds to the strain distribution along the FRP plate at a certain load value.It is observed that when the load is lower than 13.7kN,the strains in the FRP plate decrease quickly with the distance from the loaded end,which can be ascribed to much smaller axial stiffness of the bonded FRP plate with respect to that of the concrete prism.Prior to initial debonding,the increase of applied load will cause the curve to shift upward.In this situation,there is no inter-f FR 407ment as the circles shown in ig.the e ternal loadacial crack between the P plate and the concreteTransactions of Tianjin University V ol.16No.62010——prism and the stresses are transferred from the FRP plate to the concrete by the shear deformation of the adhesive.However,from the curves corresponding to the load val-ues beyond 13.7kN,the shape of the curve starts to change and the slope of the curve near the loaded end tends to decrease due to interfacial debonding failure.Since the slope of the curve determines the rate of strain change in the FRP plate,which is proportional to the shear stress at the bottom of the FRP plate,the decrease of the slope represents shear softening at the debonded interface.As the load increases,the interfacial debonding tends to propagate towards the free end of the FRP plate,which can be indicated by the shifting of strain distribu-tion curves towards the free end of the FRP plate.After the external load reaches 15.59kN,the maximum strain in the FRP plate seems to remain approximately constant,indicating that unstable debonding occurs.Fig.4Strain variations at different loading values for speci-Fig.4men B1-60-102.2Effe ct of immersing tim e and conce ntra tion on com pr essive stren gth of concreteTo investigate the correlation between compressive strength of concrete and concentration or immersing time,concrete cubes were immersed in the same solu-tions as the concrete prisms and for the same time.After taken out and totally dried in the atmosphere,the cubes were tested to obtain the compressive strength which was correlated with the immersing time and chloride concen-tration,as shown in Fig.5.From Fig.5(a ),the compressive strength of concrete increased by 57.5%of the standard compressive strength (standard curing for 28d )after being cured for 380d in the atmosphere.When the cubes were cured in the salt solutions,the compressive strength increased linearly from 27.2MPa to 32MPa along with the immersing time.Due to the incompleteness of hydration of cement at the early stage,the strength of concrete increased with curing age and immersing time.Moreover,the hydrationcan be accelerated when the cube was immersed in water.Fig.5(b )shows that there is little correlation between concentration and compressive strength,indicating that the concentration of Cl -has imperceptible effect on the strength of concrete.(a)Concrete in10%solution(b)Concrete immersed for 90dFig.5Correlation between immersing time/concen tration an d compressive strength of concrete2.3Effect of imm ersin g time and chloride conce n-tration on initia l and ultimate debonding load Based on test results,the correlations between im-mersing time and initial debonding load (P i )or ultimate load (P ult )are plotted in Fig.6(a ).When the immersing time is less than 30d,P i and P ult decrease with the im-mersing time due to the degradation of adhesive in the salt solutions [18].In the cases with immersing time of 30d to 90d,P i and P ult both increase with the immersing time because of the increase of concrete strength result-ing from further hydration of cement.At this stage,the degradation of the adhesive becomes a secondary factor.After 90d,P i and P ult decrease again with the immersing time due to the degradation of both the adhesive and con-crete.Fig.6(b)shows the correlation between the con-centration,P i and P ult .According to the test results,the concentration of chloride seems to have little effect on the initial and ultimate debonding loads.Further experi-ments on specimens with a longer corrosion time are needed to clarify this effect.408PAN Jinlong et al:Effect of Chloride Content on Bond Behavior Between FRP and Concrete——(a)Concrete in 10%solution(b)Concrete immersed for 90dFig.6Correlation between immersing time/concentrationan d load2.4Effe ct of immersing tim e and conce ntra tion on interfa cial fracture ener gyIn most existing models,the FRP/concrete bond ca-pacity can be expected from the interfacial fracture en-ergy as well as FRP stiffness,thickness and length,etc.According to the model proposed by T ljsten [19],the in-terfacial fracture energy G F can be given by2u l t F 2P P P(1)2P G E b t α+=(1)where E P is the Young ’s modulus of FRP;α=E P t P b P /(E C t C b C )(E C is the Young ’s modulus of concrete );b P ,b C are the width of the FRP plate and concrete prism respec-tively;t P is the thickness of the FRP plate;t C is the depth of the concrete prism.G F for each specimen can be calcu-lated from Eq.(1).On the other hand,Pan et a l [20]proposed that the bond capacity is mostly related to the concrete surface tensile strength (f t ).And the general relationship between G F (N/mm)and f t is assumed to take the following form:F t bG af =(2)where a,b are constant parameters;f t can be calculated bycompressive strength of concrete (f c )with empirical formula;and G F can be calculated by Eq.(1).A database of 25test results from direct shear test is employed to obtain the constants in Eq.(2)through the approach of least squares fitting.Based on the theory of ,f then calculated as a=0.387,and b=0.622.Hence,the resulting empirical equation for G F is0.622F t 0.387G f =(3)According to Eq.(1)and Eq.(3),the ratio of the predicted fracture energy (calculated by Eq.(3))to the experimental interfacial fracture energy (calculated by Eq.(1))can be figured out,as shown in Fig.7.Fig.8shows the correlation between G F and the immersing time,which is similar to that between P ult and the im-mersing time.G F decreases at the initial stage because of the deterioration of adhesive,and increases appreciably during 30d to 90d due to the hydration of cement,and thereafter decreases again until 120d as a result of the degradation of the adhesive and concrete.Since the con-centration of Cl -has little effect on the concrete strength and the ultimate bond capacity between FRP and con-crete,it also shows little correlation with the interfacial fracture energy.Fig.7Comparison of fracture energy from empirical equa-tion and experimental resultFig.8Correlation between immersing time and G F3ConclusionsIn this paper,direct shear test was conducted to in-vestigate the effect of chloride content on the bond be-havior between concrete and the FRP plates.Based on test results,the following conclusions can be drawn.(1)The concrete compressive strength increases f y N 409multiple nonlinear regressions the values o constants aresigni icantl with the immersing time in the aCl solu-Transactions of Tianjin University V ol.16No.62010——tions.The concentration of the chloride ions has little effect on the compressive strength of concrete.(2)Both the initial debonding load (P i )and ulti-mate debonding load (P ult )show a small decrease due to the degradation of the adhesive in the NaCl solution at the early stage.Then,both of them increase with the im-mersing time due to further hydration of cement.Finally,P i and P ult decrease with the immersing time because of the degradation of the adhesive and concrete in severe conditions.(3)Based on test results,the correlation between G Fand the immersing time shows the same trend as that be-tween P i (or P ult )and immersing time.The interfacial fracture energy has little correlation with the concentra-tion of Cl -in the NaCl solution.Referen ces[1]Meier U,Deuring M,Me ier H et a l.Strengthening ofstructures with CFRP laminates:Research and applications in Switzerland [J].Advanced Composite Materials in Bridges and Structures,1992,58(3):33-77.[2]Ritchie P A,Thomas D A,Lu L W et al.External strength-ening of concrete beams using fiber-reinforced plastics [J].ACI Struct J,1991,88:490-500.[3]Saadatmanesh H,Ehsani M R.RC beams strengthenedwith GFRP plates (I):Experimental study [J].J Struct Eng,1991,117(11):3417-3433.[4]Almusallam A A,Al-Gahtani A S,Rasheeduzzafar A R.Effect of reinforcement corrosion on bond strength[J].Construction and Building Materials,1996,10(2):123-129.[5]Al-Sulaimani G J,Kaleemullah M,Basunbul I A et al.Influence of 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