Letrozole_LCMS_12854_MedChemExpress
高效液相色谱法检测盐酸度洛西汀肠溶胶囊中α-萘酚杂质
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高效液相色谱法检测盐酸度洛西汀肠溶胶囊中α-萘酚杂质隋海山;戚威;王立娟【摘要】目的建立测定盐酸度洛西汀肠溶胶囊中α-萘酚杂质含量的高效液相色谱(HPLC)法.方法采用岛津-GL Inertsil CN-3液相色谱柱(250 mm×4.6 mm,5μm),流动相为乙腈-正丁醇-磷酸缓冲液(13∶17∶70),流速为1.0 mL/min,检测波长230 nm,柱温为40℃.结果α-萘酚含量在8 × 10-4~8×10-3μg范围内与峰面积呈良好线性关系(r=0.997 6),平均回收率为99.08%,RSD为0.89%(n=12).结论该方法专属性强、耐用性好、准确度高,可以控制盐酸度洛西汀肠溶胶囊中α-萘酚的含量.【期刊名称】《中国药业》【年(卷),期】2015(024)024【总页数】3页(P156-158)【关键词】高效液相色谱法;盐酸度洛西汀;α-萘酚;含量测定【作者】隋海山;戚威;王立娟【作者单位】山东省潍坊市食品药品检验检测中心,山东潍坊261041;山东省潍坊市食品药品检验检测中心,山东潍坊261041;山东省潍坊市红十字中心血站,山东潍坊261041【正文语种】中文【中图分类】R927.2;R971+.43高效液相色谱(HPLC)法是目前药物分析中常用的色谱分离、分析技术,具有较高的分析速度及分离效率,且具有检测灵敏度较高、适用测定范围广、样品处理操作简单、回收率高等特点。
随着现代质谱、核磁共振波谱等色谱技术的日益成熟及色谱联用技术的发展,HPLC法在药物制剂分析中的应用越来越广泛[1-2]。
因此,笔者通过建立HPLC法对盐酸度洛西汀肠溶胶囊中所含有的特殊杂质α-萘酚进行分离分析,控制药物中杂质α-萘酚的含量,以减少药物中所含杂质对人体造成的损害。
Aglient 1260型高效液相色谱仪(安捷伦<中国>科技有限公司);DZF-150型恒温真空干燥箱(郑州长城科工贸有限公司);KQ5200DE型数控超声波清洗器(昆山市超声仪器有限公司);PT25S型电子分析天平(赛多利斯科学仪器有限公司);ZF-20C型暗箱式紫外分析仪(上海和勤科学分析仪器有限公司);BSZ-160F型电脑自动部分收集器(上海精科实业有限公司)。
靶向代谢组学检测物汇总表
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靶向代谢组学检测物汇总表上海鹿明生物科技有限公司靶向代谢组学检测物汇总表10大类 145种代谢物鹿明生物· 代谢部2018-9目录靶向代谢组学检测物汇总表 (2)1.胆汁酸(15种)-LCMS (2)2.胆固醇类物质-LCMS(12种) (2)3.神经递质类物质-LCMS(27种) (3)4.常见氨基酸-GCMS(20种) (4)5.羧酸类物质-LCMS(7种) (4)6.植物次级代谢物-LCMS(27种) (5)7.短链脂肪酸-GCMS(7种) (6)8.嘌呤代谢相关物质-LCMS(GCMS)(14种) (6)9.木质素代谢途径化合物-LCMS(9种) (7)10.糖类-GCMS(单糖或二糖,6种) (7)靶向代谢组学检测物汇总表1.胆汁酸(15种)-LCMS中文名英文名CAS号分子式分子量胆酸Cholic acid 81-25-4 C24H40O5408.6 鹅去氧胆酸Chenodeoxycholic acid 474-25-9 C24H40O4392.6 去氧胆酸Deoxycholic acid 83-44-3C24H40O4392.6 石胆酸Lithocholic acid 434-13-9 C24H40O3376.6 熊脱氧胆酸Ursodeoxycholic acid 128-13-2 C24H40O4392.6 甘氨胆酸Glycocholic acid 475-31-0 C26H43NO6465.6 甘氨鹅脱氧胆酸Glycochenodeoxycholic acid 640-79-9 C26H43NO5449.6 甘氨脱氧胆酸Glycodeoxycholic acid 360-65-6 C26H43NO5449.6 甘氨石胆酸Glycocholic acid 475-31-0 C26H43NO6465.6 甘氨熊脱氧胆酸Glycoursodeoxycholic acid 64480-66-6 C26H43NO5449.6 牛磺胆酸 Taurocholic acid 81-24-3 C26H45NO7S 515.7 牛磺鹅脱氧胆酸T aurochenodeoxycholic acid 516-35-8 C26H45NO6S 499.7 牛磺脱氧胆酸Tauroursodeoxycholic acid 14605-22-2 C26H45NO6S 499.7 牛磺石胆酸Taurolithocholic acid 516-90-5 C26H45NO5S 483.7 牛磺熊脱氧胆酸Tauroursodeoxycholic acid 14605-22-2 C26H45NO6S 499.72.胆固醇类物质-LCMS(12种)英文名CAS号分子式分子量Cholesterol 57-88-5 C27H46O 386.7 25-hydroxycholesterol-3-sulfate 884905-07-1 C27H46O5S 482.7 22R-Hydroxycholesterol 17711-16-9 C27H46O2402.725-hydroxycholesterol 2140-46-7 C27H46O2402.727-hydroxycholesterol 20380-11-4 C27H46O2402.724-Hydroxycholesterol 474-73-7 C27H46O2402.724,25-Epoxy-cholesterol 77058-74-3 C27H44O2400.67beta-hydroxycholesterol 566-27-8 C27H46O2402.74beta-hydroxycholesterol 17320-10-4 C27H46O2402.7 7-ketocholesterol 566-28-9 C27H44O2400.6 7alpha-hydroxycholesterol 566-26-7 C27H46O2402.7 cholesterol 3-sulfate 2864-50-8 C27H48NaO4S 491.73.神经递质类物质-LCMS(27种)中文名英文名CAS号分子式分子量3,4-二羟基苯基乙酸3,4-dihydroxyphenylacetic acid 102-32-9 C8H8O4168.1 3-羟基邻氨基苯甲酸3-hydroxyanthranilic acid 548-93-6 C7H7NO3153.1 5-羟色胺5-hydroxytryptamine 50-67-9 C10H12N2O 176.2 5-羟基吲哚乙酸5-hydroxyindoleacetic acid 54-16-0 C10H9NO3191.2 5-羟色氨酸5-hydroxytryptophan 56-69-9 C11H12N2O3220.2 α-酮戊二酸Alpha-ketoglutaric acid 328-50-7 C5H6O5146.1多巴胺Dopamine 51-61-6 C8H11NO2153.2 γ-氨基丁酸Gamma-aminobutyric acid 56-12-2 C4H9NO2103.1谷氨酸Glutamic acid 56-86-0 C5H9NO4147.1 谷氨酰胺Glutamine 61348-28-5 C10H18N2O5246.3 谷胱甘肽Glutathione 70-18-8 C10H17N3O6S 307.3犬尿酸Kynurenic acid 492-27-3 C10H7NO3189.2 犬尿氨酸Kynurenine 343-65-7 C10H12N2O3208.2 左旋多巴Levodopa 59-92-7 C9H11NO4197.2 L-苯丙氨酸L-phenylalanine 673-31-4 C10H13NO2179.2 L-酪氨酸L-tyrosine 70642-86-3 C14H19NO5281.3 N-乙酰5-羟色胺N-acetyl serotonin 1210-83-9 C12H14N2O2218.3 鸟氨酸Ornithine 70-26-8 C5H12N2O2132.2 苯乙胺Phenylethylamine 64-04-0 C8H11N 121.2琥珀酸Succinic acid 110-15-6 C4H6O4118.1色胺Tryptamine 61-54-1 C10H12N2160.2色氨酸Tryptophan 5241-64-5 C16H20N2O4304.3色醇Tryptophol 526-55-6 C10H11NO 161.2酪胺Tyramine 51-67-2 C8H11NO 137.2 香草扁桃酸Vanillylmandelic acid 55-10-7 C9H10O5198.2 去甲肾上腺素Norepinephrine 51-41-2 C8H11NO3169.2 吲哚-3-甲醛Indole-3-carboxaldehyde 487-89-8 C9H7NO 145.24.常见氨基酸-GCMS(20种)中文名英文名CAS号缩写分子式分子量酪氨酸Tyrosine 70642-86-3 Tyr C14H19NO5281.3 缬氨酸Valine 7004-03-7 Val C5H11NO2117.1 苯丙氨酸Phenprobamate 673-31-4 Phe C10H13NO2179.2 丝氨酸Serine 302-84-1 Ser C3H7NO3105.1 谷氨酰胺Glutamine 61348-28-5 Gln C10H18N2O5246.3 亮氨酸Leucine 3588-60-1 Leu C14H19NO4265.3 天冬酰胺Asparagine 70-47-3 Asn C4H8N2O3132.1 组氨酸Histidine 71-00-1 His C6H9N3O2155.2 脯氨酸Dl-proline 609-36-9 Pro C5H9NO2115.1 半胱氨酸Cysteine 52-90-4 Gys C3H7NO2S 121.2 异亮氨酸Isoleucine 7004-09-3 Ile C6H13NO2131.2 谷氨酸Glutamic acid 56-86-0 Glu C5H9NO4147.1 苏氨酸Threonine 72-19-5 Thr C4H9NO3119.1 天冬氨酸Aspartic acid 6899-03-2 Asp C4H7NO4133.1 色氨酸Tryptophan 5241-64-5 Try C16H20N2O4304.3 赖氨酸Lysine 56-87-1 Lys C6H14N2O2146.2 甘氨酸Glycine 56-40-6 Gly C2H5NO275.1 甲硫氨酸Methionine 59-51-8 Met C5H11NO2S 149.2 丙氨酸Alanine 338-69-2 Ala C3H7NO289.1 精氨酸Arginine 74-79-3 Arg C6H14N4O2174.25.羧酸类物质-LCMS(7种)中文名英文名CAS号缩写分子式分子量草酸Oxalic acid 144-62-7 OA C2H2O490.0 丙酮酸Pyruvic acid 127-17-3 PA C3H4O388.1 棕榈酸Palmitic acid 57-10-3 Pal C16H32O2256.4 油酸Oleic acid 112-80-1 Ole C18H34O2282.5 亚油酸Linoleic acid 60-33-3 Lin C18H32O2280.5 愈伤酸Traumatic Acid 6402-36-4 Tra C12H20O4228.3 亚麻酸Linolenic acid 463-40-1 Lino C18H30O2278.46.植物次级代谢物-LCMS(27种)类别中文名英文名CAS号分子式分子量植物激素Phytohormones茉莉酸(+/-)-Jasmonic acid 3572-66-5 C12H18O3210.3 水杨酸Salicylic acid 69-72-7 C7H6O3138.1 生长素Indoleacetic acid 87-51-4 C10H9NO2175.2 脱落酸Abscisic acid 14375-45-2 C15H20O4264.3 反式玉米素Trans-Zeatin 1637-39-4 C10H13N5O219.24 N-(3-吲哚乙酰基)-L-丙氨酸N-(3-Indolylacetyl)-L-alanine 57105-39-2C13H14N2O3246.266 1-氨基环丙烷-1-羧酸1-AminocyclopropanecarboxylicAcid22059-21-8 C4H7NO2101.105生物碱Alkaloids加兰他敏Galanthamine 357-70-0 C17H21NO3287.4 石蒜胺Lycoramine 21133-52-8 C17H23NO3289.4 石蒜碱Lycorine 476-28-8 C16H17NO4287.3 降孤挺花啶Norbelladine C15H17NO3259.3 4'-o-methylnorbelladine 4579-60-6 C16H19NO3273.3类黄酮Flavonoids 大豆黄素Daidzein 486-66-8 C15H10O4254.2 白杨素Chrysin 480-40-0 C15H10O4254.2 异甘草素Isoliquiritigenin 961-29-5 C15H12O4256.3 乔松素Pinocembrin 480-39-7 C15H12O4256.3 芒丙花素Formononetin 485-72-3 C16H12O4268.3 芹菜素Apigenin 520-36-5 C15H10O5270.2 高良姜素Galangin 548-83-4 C15H10O5270.2 染料木素Genistein 446-72-0 C15H10O5270.2 木犀草素Luteolin 491-70-3 C15H10O6286.2 表儿茶素(-)-Epicatechin 490-46-0 C15H14O6290.3 儿茶素(+)-Catechin 154-23-4 C15H14O6290.3 桑色素Morin 480-16-0 C15H10O7302.2 异鼠李素Isorhamnetin 480-19-3 C16H12O7316.3 牡荆素Vitexin 3681-93-4 C21H20O10432.4 芦丁Rutin 153-18-4 C27H30O16610.57.短链脂肪酸-GCMS(7种)中文名英文名CAS号分子式分子量乙酸Acetic Acid97-67-6 C2H4O260.05丙酸Propionic acid69-93-2 C3H6O274丁酸Butyric Acid68-94-0 C4H8O288.11戊酸Pentanoic acid70-18-8 C5H10O2102.13己酸Hexanoic Acid58-63-9 C6H12O2116.16异丁酸Isobutyric acid58-96-8 C4H8O288.11异戊酸Isovaleric acid3868-31-3 C5H10O2102.138.嘌呤代谢相关物质-LCMS(GCMS)(14种)中文名英文名CAS号分子式分子量L-苹果酸L-Malic acid 97-67-6 C4H6O5134.1 尿酸Uric acid 69-93-2 C5H4N4O3168.1 次黄嘌呤Hypoxanthine 68-94-0 C5H4N4O 136.1 谷胱甘肽Glutathione 70-18-8 C10H17N3O6S 307.3 肌苷Inosine 58-63-9 C10H12N4O5268.2 尿苷Uridine 58-96-8 C9H12N2O6244.2 8-羟基鸟苷8-Hydroxyguanosine 3868-31-3 C10H13N5O6299.2 8-羟基-2'-脱氧鸟苷8-Hydroxy-2′-deoxyguanosine 88847-89-6 C10H13N5O5283.2 黄嘌呤Xanthine 69-89-6 C5H4N4O2152.1 胞嘧啶Cytosine 71-30-7 C4H5N3O 111.1 吲哚-3-乳酸Indole-3-lactic acid 1821-52-9 C11H11NO3205.2 鞘氨醇D-erythro-Sphingosine 123-78-4 C18H37NO2299.5 腺苷Adenosine 58-61-7 C10H13N5O4267.2 5'-一磷酸腺苷Adenosine 5'-monophosphate 61-19-8 C10H14N5O7P 347.29.木质素代谢途径化合物-LCMS(9种)中文名英文名CAS号分子式分子量肉桂酸Cinnamic acid 140-10-3 C9H8O2148.161 咖啡酸Caffeic acid 331-39-5 C9H8O4180.159 阿魏酸Ferulic acid 1135-24-6 C10H10O4194.186 芥子酸Sinapic acid 7362-37-0 C11H12O5224.212 松柏醇Coniferyl alcohol 438-35-5 C10H12O3180.203 芥子醇Sinapyl alcohol 537-33-7 C11H14O4210.229 松柏醛Coniferyl aldehyde 458-36-6C10H10O3178.187 芥子醛Sinapaldehyde 4206-58-0 C11H12O4208.213 对香豆酸P-coumaric acid 501-98-4 C9H8O3164.1610.糖类-GCMS(单糖或二糖,6种)中文名英文名CAS号分子式分子量葡萄糖glucose50-99-7 C6H12O6180.16果糖fructose57-48-7 C6H12O6180.16半乳糖Galactose10257-28-0 C6H12O6180.16乳糖lactose14641-93-1 C12H22O11342.3麦芽糖maltose69-79-4 C12H22O11342.3海藻糖Trehalose99-20-7 C12H22O11342.3。
替卡格雷原料药的合成检索报告
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化学反应式(五)
三、合成检索报告
三、合成检索报告
反应式(五)检索的文献
① LEK PHARMACEUTICALS D.D.; MARAS, Nened; ZUPANCIC, Borut WO2013/37942, 2013, A1
化学反应式(六)
三、合成检索报告
三、合成检索报告
反应式(六)检索的文献
三、合成检索报告
三、合成检索报告
反应式(七)检索的文献
① LEK Pharmaceuticals d.d.; The designation of the inventor has not yet been filed EP2586773, 2013, A1 ② LEK PHARMACEUTICALS D.D.; ZUPANCIC, Borut; MARAS, Nenad; STERK, Damjan. WO2013/60837, 2013, A1
① CHEMO RESEARCH, S.L.; RASPARINI, Marcello; PIATEK, Anna Maria; POWLES, Katharine Ann; CARCONE, Luca; D'ARIENZO, Giuseppe WO2014/154908, 2014, A1
化学反应式(七)
替卡格雷原料药的合成 检索报告
报告目录
1
替卡格雷简介
2
使用的检索工具
3
合成检索报告
一、替卡格雷简介
替卡格雷(Ticagrelor)属于环戊基三唑并嘧啶类 化合物,是由美国阿斯利康(AstraZeneca)公司研发 的一种新型的、具有选择性的小分子抗凝血药。该 药能可逆性地作用于血管平滑肌细胞(VSMC)上的嘌 呤2受体亚型P2Y12,对ADP引起的血小板聚集有 明显的抑制作用,且口服使用后起效迅速,因此能 有效改善急性冠心病患者的症状。而因替卡格雷的 抗血小板作用是可逆的,其对于那些需在先期进行 抗凝治疗后再行手术的病人尤为适用。
洛伐他汀
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洛伐他汀发酵培养基配方优化及15L罐放大作者:作者:吴波陈长华* 杨琳作者单位:华东理工大学生物反应器工程国家重点实验室,上海200237 来源:医学期刊 / 药学收藏本文章【摘要】利用响应面方法对土曲霉生产洛伐他汀的培养基进行了优化,使用两水平因子实验对培养基中的碳、氮源组分:葡萄糖、豆粕、蛋白胨、麦精和硝酸钠对洛伐他汀效价的影响进行分析,发现主要的影响因素为葡萄糖和豆粕。
通过进一步中心组合实验,考察葡萄糖和豆粕浓度对菌浓、效价、残糖浓度、单位菌体产量(YP/X)和得率(YP/S)的作用。
并通过引进残糖浓度为参考,得到最优的葡萄糖和豆粕配比分别为22%和5%,结果比对照提高了17%。
同时在15L发酵罐上放大,确定最适初始葡萄糖浓度为21%,效价为7.34g/L。
【关键词】响应面设计法;洛伐他汀;土曲霉;发酵Optimization of medium components forlovastatin production and scale up in 15L bioreactorWu Bo, Chen Chang-hua and Yang Lin(State Key Laboratory of Bioreactor Engineering, East China University ofScience and Technology, Shanghai 200237)ABSTRACT Response surface design method was used to optimize the medium components for lovastatin produced by Aspergillus terreus. Effects of glucose, soybean meal, peptone, malt extract and NaNO3 on lovastatin productivity were evaluated using a 2-level factorial design. Among the components investigated, glucose and soybean meal played important roles in lovastatin production. A central composite design was used to review the effects of glucose and soybean meal to concentration of biomass, lovastation, and residual glucose respectively, as well as YP/X and YP/S. The optimized concentrations of glucose and soybean meal were 22% and 5% respectively, by using residual glucose concentration as a reference, and the optimized medium resulted in a significant increase of lovastatin yield by 17%, as compared with the original one. It was concluded that the optimal concertration of glucose was about 21% and the lovastatin yield was 7.34g/L.KEY WORDS Response surface design; Lovastatin; Aspergillus terreus; Fermentation洛伐他汀(lovastatin)是第一个经FDA批准上市的降血脂他汀类药物,由于其竞争性的抑制了体内胆固醇合成的关键酶-羟甲基戊二酰辅酶A还原酶(HMG)的活性,从而起到降低血液中胆固醇含量的作用。
LC_MS_MS法测定人血浆中罗红霉素的血药浓度
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Chin JMAP, 2008 October, Vol. 25 No. 5 中国现代应用药学杂志 2008年 10月第 25卷第 5期
王试剂厂 ) ; 甲酸 、乙醚和碳酸钠为分析纯 (沈阳化学试剂 厂 ) ;空白血浆由沈阳中心血站提供 。 2 方法 2. 1 试验条件 2. 1. 1 色谱条件 色谱柱为 D iamonsil C18柱 (150 mm ×4. 6 mm , 5μm ) ;流动相为甲醇 2水 2甲酸 (75∶25∶0. 5) ,流速为 0. 5 mL ·m in - 1 ,柱温 :室温 。 2. 1. 2 质谱条件 ESI离子源 ;源喷雾电压为 4. 0 kV;加热 毛细管温度为 300 ℃;鞘气 (N2 )压力 25 A rb;辅助气 (N2 )压 力 5 A rb;碰撞气 (A r)压力 1. 2 mTorr;罗红霉素和克拉霉素 的碰撞诱导解离 (C ID )电压都为 25 eV;正离子方式检测 ;扫 描方式为选择反应监测 ( SRM ) ,用于定量分析的离子反应分 别为 m / z 837. 5 (m / z 679. 3 罗 红 霉 素 ) 和 m / z 748. 5 (m / z 158. 1 (克拉霉素 ) ;扫描时间为 0. 3 s。 2. 2 样品的处理方法 2. 2. 1 样品的预处理 用肝素抗凝的负压真空离心管取全 血 2 mL ,上下震荡 3次 ,以 5 000 r·m in - 1离心 5 m in,分离上 层血浆 ,立即置于冰箱 , - 20 ℃贮存 。 2. 2. 2 血浆样品的处理 向 50μL血浆中分别加入 50μL内 标溶液 (克拉霉素 10μg·mL - 1 )和 0. 05 mol·L - 1 Na2 CO3 30 μL,混匀 ;加 1 mL提取溶剂乙醚 ,涡流混合 1 m in,往复振荡 10 m in (180次 ·m in - 1 ) ,离心 5 m in ( 4 000 r·m in- 1 ) ,分取上层 有机相于另一试管中 ,于 40 ℃空气流下吹干 ,残留物加入 1 mL 流动相溶解 ,涡流混合 ,取 20μL进行 LC /MS/MS分析 。
Edaravone_LCMS_15660_MedChemExpress
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=====================================================================Acq. Operator : Li Shan(LCMS-02) Seq. Line : 24Acq. Instrument : HY-LCMS-02 Location : P1-C-03Injection Date : 4/9/2015 11:11:41 AM Inj : 1Inj Volume : 3.000 µlAcq. Method : D:\AGLIENT 1260\DATA\20150409\20150409 2015-04-09 09-27-50\100-1000MS+3MIN- 1.5_(0.02%FA).MLast changed : 4/9/2015 9:27:50 AM by Li Shan(LCMS-02)Analysis Method : D:\AGLIENT 1260\DATA\20150202\20150202 2015-02-02 09-14-27\100-1000MS+3MIN( 0.02%FA).M (Sequence Method)Last changed : 4/10/2015 10:50:09 AM by Li Shan(LCMS-02) (modified after loading)Method Info : Postive,MS:100-1000,Column ID:A-RP-102,40℃Catalog No : HY-B0099 Batch#15660 A-RP-132Additional Info : Peak(s) manually integratedmin0.511.522.53mAU 020040060080010001200 DAD1 B, Sig=214,4 Ref=off (D:\AGLIENT...60\DATA\20150409\20150409 2015-04-09 09-27-50\BIZ2015-409-DJL7.D)1.6712.047 2.133 2.220===================================================================== Area Percent Report =====================================================================Sorted By : Signal Multiplier : 1.0000Dilution : 1.0000Do not use Multiplier & Dilution Factor with ISTDsSignal 1: DAD1 B, Sig=214,4 Ref=offPeak RetTime Type Width Area Height Area # [min] [min] [mAU*s] [mAU] %----|-------|----|-------|----------|----------|--------| 1 1.671 MM 0.1486 1.24098e4 1391.72278 99.8061 2 2.047 MM 0.0470 12.53438 4.44282 0.1008 3 2.133 MM 0.0449 7.52121 2.78921 0.0605 4 2.220 MM 0.0591 4.05292 1.14401 0.0326Totals : 1.24340e4 1400.09882===================================================================== *** End of Report ***============================================================Acq. Operator : Li Shan(LCMS-02) Seq. Line : 24Acq. Instrument : HY-LCMS-02 Location : P1-C-03Injection Date : 4/9/2015 11:11:41 AM Inj : 1Inj Volume : 3.000 µlAcq. Method : D:\AGLIENT 1260\DATA\20150409\20150409 2015-04-09 09-27-50\100-1000MS+3MIN- 1.5_(0.02%FA).MLast changed : 4/9/2015 9:27:50 AM by Li Shan(LCMS-02)Analysis Method : D:\AGLIENT 1260\DATA\20150202\20150202 2015-02-02 09-14-27\100-1000MS+3MIN( 0.02%FA).M (Sequence Method)Last changed : 4/10/2015 10:51:15 AM by Li Shan(LCMS-02) (modified after loading)Method Info : Postive,MS:100-1000,Column ID:A-RP-102,40℃Catalog No : HY-B0099 Batch#15660 A-RP-132Additional Info : Peak(s) manually integratedmin0.511.522.53100000200000300000400000500000600000 MSD1 TIC, MS File (D:\AGLIENT 1260\DATA\20150409\20150409 2015-04-09 09-27-50\BIZ2015-409-DJL7.D) ES-API, Pos, Sca1.687MS Signal: MSD1 TIC, MS File, ES-API, Pos, Scan, Frag: 50 Spectra averaged over upper half of peaks. Noise Cutoff: 1000 counts.Reportable Ion Abundance: > 10%.Retention Mol. Weight Time (MS) MS Area or Ion1.687 10162227 176.00 I 175.00 Im/z10020030040050060070020406080100*MSD1 SPC, time=1.562:1.798 of D:\AGLIENT 1260\DATA\20150409\20150409 2015-04-09 09-27-50\BIZ2015-409-DJL7.D ES-API,Max: 447561370.9176.0 175.0*** End of Report ***。
高效液相色谱切换波长法同时测定辛夷鼻炎丸中4种成分的含量
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高效液相色谱切换波长法同时测定辛夷鼻炎丸中4种成分的含量目的:建立同时测定辛夷鼻炎丸中升麻素苷、甘草苷、5-O-甲基维斯阿米醇苷、甘草酸铵含量的方法。
方法:采用高效液相色谱切换波长法对A、B、C 3家企业共52批次辛夷鼻炎丸样品进行含量测定。
色谱柱为Kromasil C18,流动相为乙腈-0.1%磷酸,流速为1.0 mL/min,检测波长为220 nm(升麻素苷、甘草苷、5-O-甲基维斯阿米醇苷)和250 nm(甘草酸铵),柱温为30 ℃,进样量为10 μL。
结果:升麻素苷、甘草苷、5-O-甲基维斯阿米醇苷、甘草酸铵检测质量浓度线性范围分别为 6.138~122.77 ?g/mL(r=0.999 9)、2.502~50.03 ?g/mL (r=0.999 9)、5.988~119.75 ?g/mL(r=0.999 9)、12.788~255.76 ?g/mL(r=0.999 9);精密度、稳定性和重复性试验的RSD均1.5 ;理论板数以5-O-甲基维斯阿米醇苷峰计为12 000。
结果表明,其他成分对主成分测定无干扰。
2.4 线性关系考察精密吸取“2.2”项下混合对照品溶液0.125、0.2、0.5、1.0、2.0、2.5 mL,分别置于5 mL量瓶中,加入50%甲醇稀释至刻度,摇匀。
分别精密吸取10 μL注入液相色谱仪,以待测成分质量浓度为横坐标(x,μg/mL)、峰面积为纵坐标(y)绘制标准曲线,线性关系考察结果见表1。
2.5 检测限与定量限考察精密吸取“2.2.1”项下混合对照品溶液0.25、0.5、1 mL,分别置于10 mL量瓶中,加50%甲醇稀释至刻度,摇匀,进样分析。
当信噪比为3 ∶1时,得检测限;当信噪比为10 ∶1时,得定量限。
结果,升麻素苷、5-O-甲基维斯阿米醇苷、甘草苷、甘草酸铵的检测限分别为0.200、0.200、0.150、0.125 μg/mL,定量限分别为0.500、0.505、0.350、0.271 μg/mL。
LCMS检测西他沙星原料中基因毒性杂质的含量
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LC-MS检测西他沙星原料中基因毒性杂质的含量石莹1宋雪洁3李浩冬2路显锋2*1药物研究院分析所,扬子江药业集团,泰州2253212药物制剂新技术国家重点实验室,扬子江药业集团,泰州2253213质量管理部,扬子江药业集团,泰州225321摘要建立了LC-MS 法测定西他沙星中基因毒性杂质对甲苯磺酸甲酯和对甲苯磺酸乙酯含量的方法。
方法:采用Agilent Poroshell 120 EC-C18色谱柱;流动相为纯水(0.1%甲酸):甲醇(V/V)=60:40;稀释剂为乙腈(0.1%甲酸):纯水(V/V)=50:10;柱温为40℃;进样体积为5µl;流速为0.4ml/min;采用正离子模式进行扫描。
对甲苯磺酸甲酯测定浓度在0.76ng/ml~15.27ng/ml范围内,线性关系良好;对甲苯磺酸乙酯测定浓度在0.75ng/ml~15.01ng/ml范围内,线性关系良好。
对甲苯磺酸甲酯的定量限为0.0038ng;对甲苯磺酸乙酯的定量限为0.0038ng。
杂质回收率在限度浓度80%、100%和160%三个浓度水平均在90~110%之间,该方法准确度良好。
该方法适用于西他沙星原料中对甲苯磺酸甲酯和对甲苯磺酸乙酯的检测。
西他沙星(sitafloxacin)是日本第一制药有限公司继左氧氟沙星后开发出的一种强力广谱新氟喹诺酮类抗菌剂,该药对革兰氏阳性球菌,革兰氏阴性菌以及厌氧菌的抗菌活性是左氧氟沙星的4~32倍,同时对肺炎球菌DNA 促旋酶和拓扑同功酶有双重抑制作用。
临床表现有极广的抗菌谱,特别是对呼吸道的病菌有极强的抗菌活性。
因西他沙星的一个起始物料为对甲苯磺酸盐,在后续反应中对甲苯磺酸若有残留,可能会与溶剂甲醇、乙醇反应生成具有基因毒性的杂质—对甲苯磺酸甲酯和对甲苯磺酸乙酯,故采用LC-MS法对产品中的对甲苯磺酸甲酯/乙酯进行控制。
1、实验部分1.1仪器与试药Agilent 1200液相色谱仪(美国安捷伦公司);Agilent 6460三重串联四极杆质谱仪(美国安捷伦公司);XP205型电子天平(瑞士梅特勒托利多公司)。
羟氯喹体内代谢物-概述说明以及解释
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羟氯喹体内代谢物-概述说明以及解释1.引言在1.1 概述部分,我们将简要介绍羟氯喹及其代谢物的研究背景和重要性。
羟氯喹是一种广泛用于治疗疟疾和类风湿关节炎的药物,近年来也被广泛应用于新型冠状病毒感染的治疗中。
羟氯喹在体内通过代谢产生不同的代谢物,这些代谢物可能具有重要的药理作用,对药物疗效和副作用产生影响。
因此,对羟氯喹代谢物的研究具有重要意义,可以深化对羟氯喹药理作用的理解,为临床应用提供更有效的指导,同时也为新药研发和治疗策略的制定提供参考。
本文将系统回顾羟氯喹体内代谢物的研究进展,探讨其在药理学上的意义和未来研究方向。
1.2 文章结构文章结构部分是对整个文章内容的一个简要概括,包括文章的各个章节和各个部分的主要内容和重点。
在这里,可以简要介绍文章的主要结构和内容安排,让读者在阅读之前有一个整体的了解。
具体内容可以包括每个章节的标题和主要内容概述,如引言部分介绍了羟氯喹的基本信息和研究背景,正文部分包括了羟氯喹的药理作用和在体内的代谢过程,结论部分对文章进行了总结和展望未来研究方向等。
这样的文章结构部分可以让读者更好地理解文章的内在逻辑和组织,帮助读者更好地把握整个文章的内容和主题。
1.3 目的羟氯喹是一种常用的抗疟药物,近年来也被广泛用于治疗风湿性关节炎和类风湿性关节炎等自身免疫性疾病。
在羟氯喹的体内代谢过程中,会生成一系列代谢物,这些代谢物可能具有更广泛的生物活性和潜在的药理作用。
因此,本文旨在系统总结羟氯喹体内代谢物的生成途径、生物活性和潜在应用,并展望未来的研究方向,以期为进一步深入了解和开发羟氯喹的药理作用提供参考。
通过对羟氯喹代谢物的研究,有望为拓展其在药物治疗领域的应用提供新的思路和可能性。
2.正文2.1 羟氯喹的药理作用羟氯喹是一种抗疟药物,主要用于治疗疟疾和风湿性关节炎。
其作用机制主要包括两个方面:2.1.1 作用机制羟氯喹能够通过干扰寄生虫对人体红细胞的侵染和生长,从而达到治疗疟疾的效果。
地奥司明中吡啶含量测定研究(定稿)
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地奥司明中吡啶含量测定方法研究报告委托单位:完成人:研究单位:完成时间:目录1 实验条件与方法 (2)1.1 仪器与试剂 (2)1.1.1 仪器 (2)1.1.2 试剂 (2)1.2 色谱条件 (2)1.3 样品制备 (2)2 结果与分析 (3)2.1 精密度试验 (3)2.2 稳定性试验 (3)2.3 线性范围、检测限、定量限 (5)2.3.1 线性范围 (5)2.3.2 检测限、定量限 (6)2.3.3 样品测定范围 (6)2.4 专属性 (7)2.5 回收率 (8)2.6 耐用性 (9)3 结论 (10)地奥司明分子式为C28H32O15,结构式见图(1),分子量608.55,英文名为Diosmin。
地奥司明外观为灰黄色或淡黄色、易吸湿粉末,几乎不溶于水,溶于二甲基亚砜,几乎不溶于乙醇,溶于稀的碱性溶液。
图1 地奥司明结构式地奥司明早在1925 年就从玄参属植物林生玄参Scrophularia nodosa中被分离,1962年首次作为一个治疗药物使用。
在欧州,地奥司明作为血管保护药剂和慢性静脉疾病治疗剂的使用已经超过30年。
地奥司明可以是天然来源或从天然产物橙皮甙经碘脱氢一步而制到。
地奥司明主要用途是被用作血管保护药剂和慢性静脉疾病治疗剂使用,是典型的黄酮类化合物。
地奥司明能降低静脉扩张性和静脉血淤滞,在微循环系统,使毛细血管壁渗透能力正常化并增强其抵抗性。
临床药理学在人体采用双盲对照研究方法,验证和定量显示药物对静脉血流动力学的作用,结果表明其具有上述药理学特性。
在人体试验中,口服以C14标记的含有地奥司明制剂后,主要是通过粪便排泄,平均有14%随尿排泄,半衰期是11小时。
药物中的残留溶剂系指在原料药或辅料的生成中、以及在制剂制备过程中使用或生产而又未能完全去除的有机溶剂。
根据国际化学品安全性纲要,以及美国环境保护机构、世界卫生组织等公布的研究结果,很多有机溶剂对环境和人体都有一定的危害,因此,为保障药物的质量和用药安全,以及保护环境,需要对残留溶剂进行研究和控制。
盐酸替罗非班有关物质方法学研究
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盐酸替罗非班有关物质方法学研究作者:刘慧英王志君来源:《维吾尔医药》2013年第06期盐酸替罗非班为一种可逆性非肽类血小板表面糖蛋白受体拮抗剂,可与肝素联用,用于心绞痛病人,同时也适用于冠脉缺血性综合征病人进行冠脉血管成形术或冠脉内斑块切除术。
本实验主要是在文献研究已确定的几种测定盐酸替罗非班有关物质的方法基础上,进一步择优,并对其进行验证,以确定最优实验方法。
通过对专属性、系统适用性、线性、定量限、检测线、精密度、溶液稳定性、耐用性、回收率进行验证,其专属性强,耐用性强,灵敏度高。
表明此方法适用于盐酸替罗非班的有关物质测定。
1 实验仪器与试药1.1 仪器岛津LC-2010AHT型高效液相色谱仪,岛津国际贸易有限公司戴安Ulti Mate3000双三元液相色谱仪(二极管阵列),戴安中国有限公司HWS12型电热恒温水浴锅,上海一恒科技有限公司岛津LC-10Avp型高效液相色谱仪,岛津国际贸易有限公司Mettler AE-100电子天平,梅特勒-托利多中国PL-2002电子天平,梅特勒-托利多中国1.2 试药辛烷磺酸钠,天津市光复精细化工研究所磷酸,天津市北联精细化学品开发有限公司乙酸钠,北京化学试剂二厂乙腈,J.T.Baker30%过氧化氢,天津市东方化工厂氢氧化钠,北京化工厂盐酸,永飞化工厂磷酸二氢钾,天津市盛奥化学试剂有限公司三乙胺,国药集团化学试剂有限公司2 实验方法2.1 色谱条件色谱柱:十八烷基硅烷键合硅胶;检测波长:226nm;流动相:乙腈-水-0.2mol/L乙酸钠(30:70:5);流速:1ml/min;进样量:10μl。
2.2专属性取盐酸替罗非班0.02g于100ml容量瓶中,加流动相溶解并稀释至刻度,取上述溶液1ml 于100ml容量瓶中,加流动相稀释至刻度,得2µg/ml样品溶液,取10µl注入液相色谱仪,记录色谱图。
色谱图见由图可知,流动相不干扰测定,盐酸替罗非班起始出峰时间为4.7分钟,有关物质能够与主峰分离,说明本法专属性强。
聚二甲基硅氧烷芯片自由酶反应器检测葡萄糖
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聚二甲基硅氧烷芯片自由酶反应器检测葡萄糖作者:仲海燕周洁余晓冬陈洪渊【摘要】应用电泳中介微分析(EMMA)技术,构建聚二甲基硅氧烷(PDMS)芯片自由酶反应器,在线检测葡萄糖(Glu),在十字形的芯片通道上,采用自制的碳纤维微电极检测葡萄糖氧化酶(GOD)催化氧化Glu生成的H2O2,并对检测电位、GOD浓度、GOD进样时间、分离电压等参数进行了优化,测定了该自由酶反应器的线性范围和检出限,考察了其重现性及稳定性。
结果表明,此自由酶反应器制作方便,操作简单,重现性好,Glu浓度在0.1~20 mmol/L之间有较好的线性关系(r=0.997),检出限为19.8 μmol/L(S/N=3)。
【关键词】自由酶反应器;葡萄糖;电泳中介微分析;聚二甲基硅氧烷芯片The Key Lab of Analytical Chemistry for Life Science, Ministry of Education, School of Chemistry and Chemical Engineering, Nanjing University, Nanjing 210093)Abstract Microfluidic enzyme based reactor could be used to detect the biomolecules with high sensitivity and selectivity. Based on the electrophoretic mediated microanalysis (EMMA) method, a new kind of free enzyme based poly(dimethylsiloxane) (PDMS) microchip was developed to detect glucose (Glu). On line catalysis reaction of Glu by glucose oxidase (GOD) was carriedout on the chip. The product H2O2 was detected using single carbon fibre cylindrical electrode. Factors influencing the separation and detection, such as detection potential, GOD concentration, GOD injection time and separation voltage, were investigated and optimized. Results showed that the peak current had a good linear relationship with Glu concentration in the range of 0.1-20 mmol/L (R=0.997). The detection limit of Glu was 19.8 μmol/L (S/N=3). In addition, the PDMS enzyme based reactor had long term stability and excellent reproducibility (RSD=2.02%, n=10). It was easy to fabricate and operate, which showed great potential application in bioanalysis.Keywords Free enzyme based microchip; Glucose; Electrophoretic mediated microanalysis; Poly(dimethylsiloxane)1 引言近年来,基于酶催化反应的微流控芯片备受关注。
金雀花根水提物和乙醇提取物对小鼠高尿酸血症的影响
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China Pharmacy 2022V ol.33No.14中国药房2022年第33卷第14期金雀花根水提物和乙醇提取物对小鼠高尿酸血症的影响Δ赵俊杰1,2*,张金娟3,张春雷1,朱勤凤1,廖尚高1#(1.贵州医科大学药学院,贵阳550025;2.贵州医科大学附属医院药剂科,贵阳550002;3.贵州医科大学基础医学院,贵阳550025)中图分类号R 965文献标志码A 文章编号1001-0408(2022)14-1694-06DOI 10.6039/j.issn.1001-0408.2022.14.06摘要目的探讨金雀花根水提物(WCS )和乙醇提取物(ECS )对小鼠高尿酸血症(HUA )的影响。
方法将昆明种小鼠随机分为正常对照组、模型组、别嘌醇组(阳性对照,5mg/kg )、苯溴马隆组(阳性对照,7.8mg/kg )和WCS 低、中、高剂量组(38、75、150mg/kg )以及ECS 低、中、高剂量组(50、100、200mg/kg ),每组10只。
除正常对照组外,其余小鼠连续7d 腹腔注射氧嗪酸钾联合灌胃次黄嘌呤建立HUA 模型。
于建模第3天,各给药组小鼠灌胃相应药物,正常对照组和模型组灌胃等体积生理盐水,每日1次,连续5d 。
称定给药期间小鼠的体质量;末次给药1h 后,计算肝、肾、脾的脏器指数,测定血清尿酸(SUA )、血尿素氮(BUN )、血肌酐(SCR )含量以及血清和肝组织中黄嘌呤氧化酶(XOD )活性;检测肝组织中XOD mRNA 和蛋白的相对表达量以及肾组织中葡萄糖转运蛋白9(GLUT 9)、尿酸转运蛋白1(URAT 1)、有机阴离子转运蛋白1(OAT 1)的相对表达量;观察肾组织的病理变化。
结果各组小鼠肝脏指数和脾脏指数差异无统计学意义(P >0.05)。
与正常对照组比较,除别嘌醇组外的各给药组小鼠的体质量和BUN 、SCR 含量差异无统计学意义(P >0.05);模型组和别嘌醇组小鼠的肾脏指数、SUA 含量均显著升高(P <0.05);模型组小鼠血清和肝组织中XOD 活性、肝组织中XOD mRNA 和蛋白的相对表达量、肾组织中GLUT 9和URAT 1蛋白的相对表达量均显著升高(P <0.05),肾组织中OAT 1蛋白的相对表达量显著降低(P <0.05)。
Riluzole_SDS_MedChemExpress
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Inhibitors, Agonists, Screening LibrariesSafety Data Sheet Revision Date:Mar.-30-2017Print Date:Mar.-30-20171. PRODUCT AND COMPANY IDENTIFICATION1.1 Product identifierProduct name :RiluzoleCatalog No. :HY-B0211CAS No. :1744-22-51.2 Relevant identified uses of the substance or mixture and uses advised againstIdentified uses :Laboratory chemicals, manufacture of substances.1.3 Details of the supplier of the safety data sheetCompany:MedChemExpress USATel:609-228-6898Fax:609-228-5909E-mail:sales@1.4 Emergency telephone numberEmergency Phone #:609-228-68982. HAZARDS IDENTIFICATION2.1 Classification of the substance or mixtureGHS Classification in accordance with 29 CFR 1910 (OSHA HCS)Acute toxicity, Oral (Category 4),H302Acute aquatic toxicity (Category 1),H400Chronic aquatic toxicity (Category 1),H4102.2 GHS Label elements, including precautionary statementsPictogramSignal word WarningHazard statement(s)H302 Harmful if swallowed.H410 Very toxic to aquatic life with long lasting effects.Precautionary statement(s)P264 Wash skin thoroughly after handling.P270 Do not eat, drink or smoke when using this product.P273 Avoid release to the environment.P301 + P312 IF SWALLOWED: Call a POISON CENTER or doctor/ physician if you feel unwell.P330 Rinse mouth.P391 Collect spillage.P501 Dispose of contents/ container to an approved waste disposal plant.2.3 Other hazardsNone.3. COMPOSITION/INFORMATION ON INGREDIENTS3.1 SubstancesSynonyms:PK 26124Formula:C8H5F3N2OSMolecular Weight:234.19CAS No. :1744-22-54. FIRST AID MEASURES4.1 Description of first aid measuresEye contactRemove any contact lenses, locate eye-wash station, and flush eyes immediately with large amounts of water. Separate eyelids with fingers to ensure adequate flushing. Promptly call a physician.Skin contactRinse skin thoroughly with large amounts of water. Remove contaminated clothing and shoes and call a physician.InhalationImmediately relocate self or casualty to fresh air. If breathing is difficult, give cardiopulmonary resuscitation (CPR). Avoid mouth-to-mouth resuscitation.IngestionWash out mouth with water; Do NOT induce vomiting; call a physician.4.2 Most important symptoms and effects, both acute and delayedThe most important known symptoms and effects are described in the labelling (see section 2.2).4.3 Indication of any immediate medical attention and special treatment neededTreat symptomatically.5. FIRE FIGHTING MEASURES5.1 Extinguishing mediaSuitable extinguishing mediaUse water spray, dry chemical, foam, and carbon dioxide fire extinguisher.5.2 Special hazards arising from the substance or mixtureDuring combustion, may emit irritant fumes.5.3 Advice for firefightersWear self-contained breathing apparatus and protective clothing.6. ACCIDENTAL RELEASE MEASURES6.1 Personal precautions, protective equipment and emergency proceduresUse full personal protective equipment. Avoid breathing vapors, mist, dust or gas. Ensure adequate ventilation. Evacuate personnel to safe areas.Refer to protective measures listed in sections 8.6.2 Environmental precautionsTry to prevent further leakage or spillage. Keep the product away from drains or water courses.6.3 Methods and materials for containment and cleaning upAbsorb solutions with finely-powdered liquid-binding material (diatomite, universal binders); Decontaminate surfaces and equipment by scrubbing with alcohol; Dispose of contaminated material according to Section 13.7. HANDLING AND STORAGE7.1 Precautions for safe handlingAvoid inhalation, contact with eyes and skin. Avoid dust and aerosol formation. Use only in areas with appropriate exhaust ventilation.7.2 Conditions for safe storage, including any incompatibilitiesKeep container tightly sealed in cool, well-ventilated area. Keep away from direct sunlight and sources of ignition.Recommended storage temperature:Powder-20°C 3 years4°C 2 yearsIn solvent-80°C 6 months-20°C 1 monthShipping at room temperature if less than 2 weeks.7.3 Specific end use(s)No data available.8. EXPOSURE CONTROLS/PERSONAL PROTECTION8.1 Control parametersComponents with workplace control parametersThis product contains no substances with occupational exposure limit values.8.2 Exposure controlsEngineering controlsEnsure adequate ventilation. Provide accessible safety shower and eye wash station.Personal protective equipmentEye protection Safety goggles with side-shields.Hand protection Protective gloves.Skin and body protection Impervious clothing.Respiratory protection Suitable respirator.Environmental exposure controls Keep the product away from drains, water courses or the soil. Cleanspillages in a safe way as soon as possible.9. PHYSICAL AND CHEMICAL PROPERTIES9.1 Information on basic physical and chemical propertiesAppearance Light yellow to yellow (Solid)Odor No data availableOdor threshold No data availablepH No data availableMelting/freezing point No data availableBoiling point/range No data availableFlash point No data availableEvaporation rate No data availableFlammability (solid, gas)No data availableUpper/lower flammability or explosive limits No data availableVapor pressure No data availableVapor density No data availableRelative density No data availableWater Solubility No data availablePartition coefficient No data availableAuto-ignition temperature No data availableDecomposition temperature No data availableViscosity No data availableExplosive properties No data availableOxidizing properties No data available9.2 Other safety informationNo data available.10. STABILITY AND REACTIVITY10.1 ReactivityNo data available.10.2 Chemical stabilityStable under recommended storage conditions.10.3 Possibility of hazardous reactionsNo data available.10.4 Conditions to avoidNo data available.10.5 Incompatible materialsStrong acids/alkalis, strong oxidising/reducing agents.10.6 Hazardous decomposition productsUnder fire conditions, may decompose and emit toxic fumes.Other decomposition products - no data available.11.TOXICOLOGICAL INFORMATION11.1 Information on toxicological effectsAcute toxicityClassified based on available data. For more details, see section 2Skin corrosion/irritationClassified based on available data. For more details, see section 2Serious eye damage/irritationClassified based on available data. For more details, see section 2Respiratory or skin sensitizationClassified based on available data. For more details, see section 2Germ cell mutagenicityClassified based on available data. For more details, see section 2CarcinogenicityIARC: No component of this product present at a level equal to or greater than 0.1% is identified as probable, possible or confirmed human carcinogen by IARC.ACGIH: No component of this product present at a level equal to or greater than 0.1% is identified as a potential or confirmed carcinogen by ACGIH.NTP: No component of this product present at a level equal to or greater than 0.1% is identified as a anticipated or confirmed carcinogen by NTP.OSHA: No component of this product present at a level equal to or greater than 0.1% is identified as a potential or confirmed carcinogen by OSHA.Reproductive toxicityClassified based on available data. For more details, see section 2Specific target organ toxicity - single exposureClassified based on available data. For more details, see section 2Specific target organ toxicity - repeated exposureClassified based on available data. For more details, see section 2Aspiration hazardClassified based on available data. For more details, see section 212. ECOLOGICAL INFORMATION12.1 ToxicityNo data available.12.2 Persistence and degradabilityNo data available.12.3 Bioaccumlative potentialNo data available.12.4 Mobility in soilNo data available.12.5 Results of PBT and vPvB assessmentPBT/vPvB assessment unavailable as chemical safety assessment not required or not conducted.12.6 Other adverse effectsNo data available.13. DISPOSAL CONSIDERATIONS13.1 Waste treatment methodsProductDispose substance in accordance with prevailing country, federal, state and local regulations.Contaminated packagingConduct recycling or disposal in accordance with prevailing country, federal, state and local regulations.14. TRANSPORT INFORMATIONDOT (US)This substance is considered to be non-hazardous for transport.IMDGUN number: 3077Class: 9Packing group: IIIEMS-No: F-A, S-FProper shipping name: ENVIRONMENTALLY HAZARDOUS SUBSTANCE, SOLID, N.O.S.Marine pollutant: Marine pollutant.IATAUN number: 3077Class: 9Packing group: IIIProper shipping name: Environmentally hazardous substance, solid, n.o.s.15. REGULATORY INFORMATIONSARA 302 Components:No chemicals in this material are subject to the reporting requirements of SARA Title III, Section 302.SARA 313 Components:This material does not contain any chemical components with known CAS numbers that exceed the threshold (De Minimis) reporting levels established by SARA Title III, Section 313.SARA 311/312 Hazards:No SARA Hazards.Massachusetts Right To Know Components:No components are subject to the Massachusetts Right to Know Act.Pennsylvania Right To Know Components:No components are subject to the Pennsylvania Right to Know Act.New Jersey Right To Know Components:No components are subject to the New Jersey Right to Know Act.California Prop. 65 Components:This product does not contain any chemicals known to State of California to cause cancer, birth defects, or anyother reproductive harm.16. OTHER INFORMATIONCopyright 2017 MedChemExpress. The above information is correct to the best of our present knowledge but does not purport to be all inclusive and should be used only as a guide. The product is for research use only and for experienced personnel. It must only be handled by suitably qualified experienced scientists in appropriately equipped and authorized facilities. The burden of safe use of this material rests entirely with the user. MedChemExpress disclaims all liability for any damage resulting from handling or from contact with this product.Caution: Product has not been fully validated for medical applications. For research use only.Tel: 609-228-6898 Fax: 609-228-5909 E-mail: tech@Address: 1 Deer Park Dr, Suite Q, Monmouth Junction, NJ 08852, USA。
流动注射化学发光法测定醋氯芬酸
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流动注射化学发光法测定醋氯芬酸刘欢;张琰图;双海军;宋馥馨【摘要】基于酸性条件下醋氯芬酸对高锰酸钾氧化甲醛产生微弱化学发光反应体系具有很强的增敏作用,且增强的发光强度在一定范围内与醋氯芬酸浓度呈良好的线性关系,结合流动注射分析技术,建立了测定醋氯芬酸的化学发光新方法.该法测定醋氯芬酸的线性范围为0.08~5.0 mg/L,检出限(3σ)为3.0×10-2mg/L,相对标准偏差(RSD)为1.7%(n=11,c=0.50 mg/L),回收率为98.1%~104.6%.该法已用于片剂和胶囊中醋氯芬酸含量的测定.【期刊名称】《分析测试学报》【年(卷),期】2016(035)004【总页数】4页(P497-500)【关键词】流动注射;化学发光;醋氯芬酸;高锰酸钾【作者】刘欢;张琰图;双海军;宋馥馨【作者单位】延安大学化学与化工学院,陕西延安716000;延安大学化学与化工学院,陕西延安716000;延安大学化学与化工学院,陕西延安716000;延安大学化学与化工学院,陕西延安716000【正文语种】中文【中图分类】O657.3;TQ460.72醋氯芬酸(Aceclofenac,ACF,结构如图1所示)别名乙酰氯芬酸,学名为2-(2,6-二氯苯胺基)苯乙酰氧基乙酸,是一种新型苯乙酸类非甾体抗炎镇痛药物,可选择性地抑制环氧化酶活性并减少前列腺素的合成,在临床上被用于治疗骨关节炎、类风湿性关节炎、强直性脊柱炎等多种疾病[1],但长期或大剂量服用往往会使人体出现腹痛、胃肠道系统失调、肝酶升高甚至引发中枢和外周神经系统疾病[2]。
故建立快速、准确、灵敏的ACF含量检测方法在临床医学及药理学研究方面具有重要意义。
ACF的测定方法主要有高效液相色谱法[3-4]、气相色谱法[5]、分光光度法[6-7]、电化学法[8-9]及毛细管电泳法[10]等。
东磊磊等[10]从优缺点、适用条件及专属性等方面对这些方法作了详细的评述。