Improved skeleton extraction and surface generation for sketch-based modeling

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浸提和超声辅助提取法对桑叶提取物抗氧化活性的影响

浸提和超声辅助提取法对桑叶提取物抗氧化活性的影响

物 :精确称取桑叶粉末 20g 加入 500mL 平底烧 含量。
瓶中,按料液比 1∶15 分别加入水、25% 乙醇、
没食子酸标准曲线的绘制 :配制浓度梯度为
50% 乙mL 的 没 食 子 酸 标 准 品
预浸泡 0.5h 后,于 50℃下超声 0.5h,超声功率 水溶液,分别取不同浓度的没食子酸标准液 1mL
桑树是我国重要的药食同源树种,其叶作为 中药材的历史悠久,具有疏风清热、清肺润燥和 清肝明目等功效[5]。大量研究表明,桑叶中含有 多酚类、生物碱、多糖和蛋白类等活性物质,其 中 多 酚 类 化 合 物 具 有 明 显 的 抗 氧 化 作 用, 而 其 他化学成分也表现出一定的抗氧化活性[6-7]。因 此,桑叶提取物直接作为抗氧化剂具有重要的开 发价值。有效的提取技术(包括提取方法、溶剂 选择等)是提高桑叶提取物的得率和抗氧化活性 的关键步骤。目前,有关桑叶的研究主要集中于 单一提取技术的工艺优化、化学成分及生理活性 方面。杨上莺等[8]优化了超声辅助乙醇提取桑叶 多酚的工艺,超声提取有效了桑叶多酚的提取效 率,但未对提取物的抗氧化活性进行研究。洪璇 等[9]优化了乙醇浸提法提取鸡桑叶多酚的工艺, 并对抗氧化能力进行测定。沈维治等[10]利用超 声辅助提取桑叶中的总多酚,并研究了桑叶总多 酚与体外抗氧化能力的相关性。然而针对提高桑 叶提取物抗氧化活性的提取技术方面的对比研究
Forest Products,Guangxi Collaborative Innovation Center for Chemistry and Engineering of Forest Products,Guangxi University for Nationalities,Nanning 530006)

响应面法优化硫酸软骨素提取的酶解工艺

响应面法优化硫酸软骨素提取的酶解工艺

响应面法优化硫酸软骨素提取的酶解工艺陈亚;徐晓燕【期刊名称】《中国生化药物杂志》【年(卷),期】2012(033)005【摘要】目的以猪喉软骨为原料,提取硫酸软骨素,优化酶解工艺条件.方法采用碱提-酶解-醇沉的方法提取硫酸软骨素,在单因素试验的基础上,通过响应面分析优化酶解工艺.结果酶解最佳工艺组合为:胰酶浓度1.0%、pH值8.6、酶解温度46℃、酶解时间2.8h.结论采用上述组合,以氨基葡萄糖含量为指标,氨基葡萄糖含量达25.94%.研究结果具有工业应用价值.%Purpose The chondroitin sulfate was isolated from pig laryngeal cartilage. The technique of enzymatic hydrolysis of chondroitin sulfate extraction was improved. Methods The chondroitin sulfate was isolated through the process of alkali extraction-enzymatic hydrolysis-alcohol precipitation. Based on the single factor tests, the technique of enzymatic hydrolysis of chondroitin sulfate extraction was improved by response surface methodology. Results To extract the chondroitin sulfate from pig laryngeal cartilage in enzymatic hydrolysis,the best combination of extracting technique was; the enzyme concentration of 1.0% ,8. 6 of pH, the temperature of 46℃ , and the timeof 2. 8 h. Conclusion The content of glu-cosamine in the chondroitin sulfate was 25. 94% after the optimization of the technique. The results can be calculated for industrial use.【总页数】4页(P548-551)【作者】陈亚;徐晓燕【作者单位】江苏省滩涂生物资源与环境保护重点建设实验室,江苏省盐城技师学院,江苏盐城224002;江苏省滩涂生物资源与环境保护重点建设实验室,江苏省盐城技师学院,江苏盐城224002【正文语种】中文【中图分类】R282.74;TQ464.1【相关文献】1.响应面法优化中性蛋白酶提取牡蛎牛磺酸酶解工艺条件 [J], 刘亚南;张志胜;佟海菊;孙克岩;宋欣2.响应面法优化鲨鱼硫酸软骨素的提取条件 [J], 张弘;谢果凰;茅大振;何斌辉;傅春燕;刘冰冰;杨文鸽3.响应面法优化鹅全骨硫酸软骨素的酶法提取工艺 [J], 谢晶;尹义捐;杨欲成;金晨钟;王双辉;卢超4.响应面法优化鹿骨多肽酶解工艺及其体外抗氧化活性 [J], 揣欣欣;郭冰洁;刘露露;牛红梅;马月;张亚丽;刘小瑜;苑广信5.响应面法优化蛋壳膜硫酸软骨素提取工艺 [J], 刘涛;张铁鹏;栾欣悦;刘贺;刘宁因版权原因,仅展示原文概要,查看原文内容请购买。

211251888_响应面优化藏羊皮胶原蛋白肽超声辅助提取工艺及其体内抗氧化活性分析

211251888_响应面优化藏羊皮胶原蛋白肽超声辅助提取工艺及其体内抗氧化活性分析

牛金鸽,吴海玥,马世科,等. 响应面优化藏羊皮胶原蛋白肽超声辅助提取工艺及其体内抗氧化活性分析[J]. 食品工业科技,2023,44(11):163−170. doi: 10.13386/j.issn1002-0306.2022060009NIU Jinge, WU Haiyue, MA Shike, et al. Optimization of Ultrasonic Assisted Extraction of Tibetan Sheep Skin Collagen Peptide by Response Surface Methodology and Its Antioxidant Activity in Vivo [J]. Science and Technology of Food Industry, 2023, 44(11):163−170. (in Chinese with English abstract). doi: 10.13386/j.issn1002-0306.2022060009· 工艺技术 ·响应面优化藏羊皮胶原蛋白肽超声辅助提取工艺及其体内抗氧化活性分析牛金鸽1,吴海玥2,马世科2,闫忠心2, *,王学江3,李 婧3,胡 蓉2,祁全青3(1.青海大学农牧学院,青海西宁 810016;2.青海大学畜牧兽医科学院,青海西宁 810016;3.青海省乡村产业发展指导中心,青海西宁 810000)摘 要:为明确超声辅助提取对藏羊皮胶原蛋白肽含量及功能活性的影响。

试验采用响应面法研究了料液比、超声功率和超声时间3个因素,确定了胶原蛋白肽最佳超声辅助提取工艺;并对藏羊皮胶原蛋白肽进行了抗氧化能力分析,模拟消化过程中的还原力和·OH 清除能力研究。

结果表明:超声辅助处理能明显提高胶原蛋白肽含量,最佳超声提取工艺为料液比1:18、超声功率220 W ,超声时间27 min ,藏羊皮胶原蛋白肽含量为30.21%±1.67%。

219525878_超声辅助低共熔溶剂提取红松树皮原花青素及动力学研究

219525878_超声辅助低共熔溶剂提取红松树皮原花青素及动力学研究

周佳悦,候艳丽,王凡予,等. 超声辅助低共熔溶剂提取红松树皮原花青素及动力学研究[J]. 食品工业科技,2023,44(14):229−236. doi: 10.13386/j.issn1002-0306.2022100070ZHOU Jiayue, HOU Yanli, WANG Fanyu, et al. Ultrasonic-Assisted Deep Eutectic Solvent Extraction of Proanthocyanidins from Korean Pine Bark and Its Kinetics[J]. Science and Technology of Food Industry, 2023, 44(14): 229−236. (in Chinese with English abstract). doi: 10.13386/j.issn1002-0306.2022100070· 工艺技术 ·超声辅助低共熔溶剂提取红松树皮原花青素及动力学研究周佳悦1,候艳丽1,王凡予1,郭庆启1,2,*(1.东北林业大学生命科学学院,黑龙江哈尔滨 150040;2.黑龙江省森林食品资源利用重点实验室,黑龙江哈尔滨 150040)摘 要:目的:对超声辅助低共熔溶剂法提取红松树皮原花青素的工艺条件进行优化,拟合提取动力学方程,旨在对红松树皮中原花青素的资源开发利用提供理论和技术参考。

方法:以原花青素得率为指标,筛选最佳低共熔溶剂体系,并进一步通过单因素结合响应面优化超声辅助低共熔溶剂提取红松树皮中原花青素的主要工艺参数。

通过提取过程中不同温度和不同时间条件下原花青素得率的变化,拟合出最佳的原花青素提取动力学模型并验证。

结果:氯化胆碱、丙三醇和水的摩尔比为1:1:4制备的低共熔溶剂为红松树皮原花青素的最佳提取溶剂;响应面法优化工艺参数条件为:液料比16 mL/g ,超声时间50 min ,超声温度55 ℃,超声功率480 W 时,红松树皮原花青素的提取效果最好,原花青素得率为4.11%;Boltzman 模型能够很好地拟合超声辅助低共熔溶剂提取原花青素动力学过程(R 2≥0.9768),模型验证值与预测值拟合度较高(R 2≥0.9442)。

响应面法优化龙须菜多糖快速溶剂萃取提取工艺及其抗炎活性研究

响应面法优化龙须菜多糖快速溶剂萃取提取工艺及其抗炎活性研究

王慧颖,刘燕飞,张敬远,等. 响应面法优化龙须菜多糖快速溶剂萃取提取工艺及其抗炎活性研究[J]. 食品工业科技,2023,44(23):110−117. doi: 10.13386/j.issn1002-0306.2023030309WANG Huiying, LIU Yanfei, ZHANG Jingyuan, et al. Optimization of Accelerated Solvent Extraction of Polysaccharides from Gracilaria lemaneiformis Using Response Surface Methodology and Anti-inflammatory Activity[J]. Science and Technology of Food Industry, 2023, 44(23): 110−117. (in Chinese with English abstract). doi: 10.13386/j.issn1002-0306.2023030309· 研究与探讨 ·响应面法优化龙须菜多糖快速溶剂萃取提取工艺及其抗炎活性研究王慧颖,刘燕飞,张敬远,杜 彬*,杨越冬*(河北省天然产物活性成分与功能重点实验室,河北秦皇岛 066004)摘 要:为了建立快速溶剂萃取技术(ASE )提取龙须菜多糖的新方法,本文以秦皇岛龙须菜为原料,利用ASE 提取龙须菜粗多糖(GLP-K ),以多糖得率为指标,采用单因素实验结合响应面试验法优化提取工艺条件。

通过傅里叶红外光谱和高效液相色谱对多糖进行结构表征;探索GLP-K 在脂多糖(LPS )诱导的RAW264.7巨噬细胞中的抗炎作用。

结果表明,快速溶剂萃取法用于龙须菜多糖提取的最佳工艺参数为提取温度70 ℃,提取时间8.5 min ,循环4次,在此条件下,多糖实验得率为9.58%±0.31%;红外光谱证实该多糖含有糖醛酸,重均分子量在4.4~747.1 kDa 之间;GLP-K 在浓度1000 μg/mL 及以下时对RAW264.7细胞增殖也无影响(P <0.001);与模型组相比,GLP-K 给药组(50、100、200、300、400、500 μg/mL )NO 的释放量显著降低43.76%~69.47%(P <0.001)。

角蛋白提取和制膜的研究

角蛋白提取和制膜的研究
羊毛中含有99%[11的角蛋白,回收利用羊毛的重点在于从中提取出角蛋白。 天然角蛋白的加工利用已经有很长的历史。随着对角蛋白的理论研究和应用研究 的开展,角蛋白粉已经广泛应用于饲料中,并且国内外有很多人正在研究利用角 蛋白开发表面活性剂、絮凝剂、氨基酸产品和系列保健品等。近年来,可生物降 解塑料和生物医学材料受到广泛的重视,如何从羊毛、禽羽毛等资源中提取角蛋 白来制备这些材料是~个重要课题。因为角蛋白膜具有生物相容性和可生物降解 性,将角蛋白用于生物移植及缝合线、绷带、分离膜和包装材料等的制备将大有 前途。
reductant solution.The result of orthogonal experiments showed that when the wool
was reduced by O.5moYL sodium thioglycolate solution(pH=lo)at 45 6Cfor 8h,the
受回归自然风气的影响,人们更加喜爱天然棉、毛、麻、丝的衣服,因为它 们不仅穿着舒适,而且没有过敏等反应。而蛋白纤维具有最好的亲和性和舒适性 以及强的吸湿性和良好的弹性,可以和天然的棉、毛、麻、丝等相媲美,用角蛋 白制造蛋白纤维将大有前途。将角蛋白溶液涂于合成纤维上形成涂层,所得到的 改性纤维将会因为其表面的那一层角蛋白涂层而具有一些蛋白纤维的优良性质。 因此,探索用角蛋白溶液对合成纤维进行涂层改性也很有意义。
highest molecular weight is 96000 and reasonable recoveray ofkeratin resulted.
Researches on how to prepare keratin membrane from the extracted keratin and the separation performance of the as-prepared membrane were also carried out.The experimental results indicated that the membranes are none porous.The Metha

响应面法优化超声辅助提取猕猴桃糖蛋白

响应面法优化超声辅助提取猕猴桃糖蛋白

Optim ization of ultrasonic extraction of kiwifruit glycoprotein by response
surface m ethodoloilY
、) ̄ NG An-na,CUI W en-hui,WU Li-2en’LI Lan-xin
(CoHege of Food Science and Technology,Hena n University of Technology,Zhengzhou 450001,Hena n , China)
猕猴桃被誉为 “水果之王” ,全世界猕猴桃科 属 植 物有 66个 品种 ,我 国有 62个 品种 】。我 国猕 猴 桃 的年 产 量 在 20万 t以上 ,但 加 工 量 只 有 11% 左右 。猕 猴桃 果实 清香 鲜美 ,酸 甜可 口 ,具有 很 高 的营养 、医疗 、观赏等价值 。猕猴桃不仅可以增进 食欲 、抗氧化 、抗老化 ,提高机体免疫能力 ,而且 能够 有效 调节 脂肪 细胞 的分 化 ,降低 血液 中的胆 固 醇 等 【2】。猕 猴 桃 果 实 含 有 17种 氨 基 酸 ,包 括 除 色 氨 酸外 的人 体必 需 的 7种 氨基 酸 ,其 中蛋 白质含 量 为 0.86% ̄1.85%、总氨基酸含量为 1O.7 l7.94 mg/g ̄ 。 糖蛋 白是 生 物体 内重 要 的生物 活性 物 质 ,在 生物 体 内起到信号传递识别 、物质运输 、刺激生长分裂等 一 系列生理活性功能 ,对人体具有增强免疫力 、抗 肿 瘤 、抗 氧 化 、降低 血糖 、血脂 等重 要作 用 。
Abstract:The response surface m ethodology was used to optim ize the key factors of extraction of

响应面优化苦参种子黄酮超声提取工艺

响应面优化苦参种子黄酮超声提取工艺

ultrasound extraction of flavonoids from Sophora flavescens seeds. The optimum technological
conditions were as follows: ratio of liquid-solid 13 ∶ 1 (mL/g), ultrasound time 105 min and
LabTech 型紫外分光光度仪:北京莱伯泰仪器 有限公司;电子天平:上海精密科技学仪器有限公
目前的研究报道认为苦参药材中主要含有生物碱 类和黄酮类成分,它们也是公认的抗菌活性成分 [5]。
司;Q6J3-W1000A 型高速万能粉碎机:天津泰斯 特仪器有限公司;GZX-9070 MBE 型数显电热鼓
ultrasound power 74 Hz. Under the optimized conditions, the predicted extraction amount of
flavonoids was 13.49 mg/g, and the verified extraction amount was 13.41 mg/g, which was
提取条件,以期为开发苦参种子黄酮类制剂产品以
准确称取粉碎至适当粒径的苦参种子干燥粉末
收稿日期:2017-06-19 基金项目:国家自然科学基金(81360686) 作者简介:徐艳丽(1992—),女,硕士研究生,研究方向为中药制剂现代化。
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粮食与油脂
2019 年第 32 卷第 2 期
5.0 g,在一定液料比条件下加入 80 % 乙醇,以一 定的功率超声提取一定时间,将提取液放置至室温 后抽滤,收集滤液即得。取适量提取液,分别加入 相应的显色试剂,通过颜色反应鉴别提取液中含有 的成分类别。 1.3.2 芦丁对照品溶液及苦参种子提取液测定波长 的选择

羟基肉桂酸的高效提取

羟基肉桂酸的高效提取

Highly effective extraction of hydroxycinnamic acids by hydrogen-bonding-functionalized ionicliquidsYunchang Fan a ,Xiaojing Li a ,Ping Shen b ,Hongxin Cai c ,⇑,Feifei Li a ,Yongxiang Wang d ,⇑aCollege of Chemistry and Chemical Engineering,Henan Polytechnic University,Jiaozuo 454003,China bSchool of Materials Science and Engineering,Henan Polytechnic University,Jiaozuo 454003,China cSchool of Physics and Electronic Information,Henan Polytechnic University,Jiaozuo 454003,China dHenan Key Laboratory of Biomolecular Recognition and Sensing,College of Chemistry and Chemical Engineering,Shangqiu Normal University,Shangqiu 476000,Chinaa r t i c l e i n f o Article history:Received 20October 2016Received in revised form 6January 2017Accepted 22January 2017Available online 25January 2017Keywords:Hydrogen-bonding-functionalized ionic liquids (HBFILs)Hydroxycinnamic acids ExtractionHydrogen-bonding interaction Hydrophobic interaction Steric hindrancea b s t r a c tIn this work,imidazolium-based ionic liquids (ILs)were used to extract hydroxycinnamic acids from water.Experimental results indicated that the ILs with CF 3SO 3Àanion had higher extraction ability for hydroxycinnamic acids because of the stronger hydrogen-bonding strength of CF 3SO 3À.The combination of cation and anion,both of which have strong hydrogen-bonding ability,generates a hydrogen-bonding-functionalized IL,1-butyl-3-(11-hydroxyundecyl)imidazolium trifluoromethanesulfonate ([C 4C 11OHim]CF 3SO 3)which has strongest hydrogen-bonding ability and strongest extraction ability for hydroxycin-namic acids.Thermodynamic analysis suggested that hydrogen-bonding interaction was the major driv-ing force;meanwhile,the influence of hydrophobic interaction and steric hindrance between ILs and hydroxycinnamic acids should be considered when interpreting the extraction behavior of ILs.The extraction ability of the ILs was strongly influenced by the aqueous pH;it decreased with increasing pH in the range of pH >p K a (dissociation constant).The stronger extraction ability of ILs at lower pH val-ues could be interpreted by the strong hydrogen-bonding interaction between ILs and the undissociated hydroxyl and carboxyl groups of the hydroxycinnamic acids.Preliminary results suggested that [C 4C 11OHim]CF 3SO 3may be applied to the process of the recovery of hydroxycinnamic acids from aque-ous media.Ó2017Elsevier B.V.All rights reserved.1.IntroductionHydroxycinnamic acids are a group of phenolic acids that are widespread in the plant kingdom with biological activities,such as antioxidant,anti-inflammatory,antimicrobial,anticancer and anti-anxiety activities [1–4]and have been widely used in the food,medicine and cosmetic industries [5].Fermentation [6,7],enzy-matic hydrolysis [8–10],acid hydrolysis [11,12]and alkaline hydrolysis [13,14]are the conventional technologies used to release hydroxycinnamic acids from plant resources.A separation process is generally required to recover hydroxycinnamic acids from fermentation broths and hydrolysates;liquid-liquid extrac-tion (LLE)is frequently used for this purpose [8,11–13,15].How-ever,traditional solvent extraction usually involves the use of volatile,irritant and flammable organic solvents,such as ethyl acetate [8,11–13],diethyl ether [12,16]and chloroform [16,17].The development of environmentally-benign solvents to replace conventional organic solvents is thus of great importance.In the past two decades,ionic liquids (ILs)which are constituted exclusively of ions and are liquid at or close to room temperature,have emerged as an environmentally friendly alternative to the volatile organic solvents due to their high thermal and chemical stability and non-volatile property [18,19].Recently,the applica-tions of ILs in the field of separation processes have attracted much attention from the scientific community and three excellent reviews have summarized the related literature [20–22].Further-more,Yu and coworkers [23]have also reported the extraction of two hydroxycinnamic acids,ferulic acid (FA)and caffeic acid (CA)with ILs,1-butyl-3-methylimidazolium hexafluorophosphate ([C 4mim][PF 6])and 1-hexyl-3-methylidazolium hexafluorophos-phate ([C 6mim][PF 6]).The results indicated that the extraction effi-ciencies of FA and CA were influenced by the pH of aqueous phase and phase volume ratio.After extraction,FA and CA in the extrac-tion phase could be retrieved quantitatively,and the ILs could be reused.Although interesting results have been obtained from Yu’s work,there are still two problems which need to be further/10.1016/j.seppur.2017.01.0571383-5866/Ó2017Elsevier B.V.All rights reserved.⇑Corresponding authors.E-mail addresses:hongxincai2013@ (H.Cai),wangyx2006@ (Y.Wang).Separation and Purification Technology 179(2017)126–134Contents lists available at ScienceDirectSeparation and Purification Technologyj o u r n a l h o m e p a g e :w w w.e l s e v i e r.c o m /l o c a t e /s ep p urelucidated:(I)PF6Àis unstable and tends to release toxic and corro-sive HF gas when contacting with water[24,25].(II)Many works [23,26–28]have illustrated that the hydrogen-bonding interaction between ILs and organic acids played an important role in the extraction processes.The BF4À-based ILs were usually selected as the ideal extractants for the extraction of organic acids due to their stronger hydrogen-bonding strength[29–33].However,BF4Àis also unstable and prone to decomposition with the release of HF when being in contact with water[25].It is necessary to develop stable IL anions with strong hydrogen-bonding strength.As reported in literature,ClO4À[34,35]and CF3SO3À[36,37]are hydrolytically stable ions and their hydrogen-bonding strength is close to that of BF4À[38,39].This suggests that ClO4À-and CF3SO3À-based ILs are the ideal alternatives to BF4À-based ones.The most widely used CF3SO3À-based IL in separationfield is1-butyl-3-methylimidazolium trifluoromethanesulfonate([C4mim]CF3SO3) [40,41].However,[C4mim]CF3SO3is miscible with water and can only be used in aqueous biphasic systems which consume large quantities of ILs(25.08–40%(wt%)[40,41]),inorganic salts (16.18%(wt%)[40])or carbohydrates(25%(wt%)[41]).The use of hydrophobic ILs in separationfield is preferable due to the low consumption of ILs[27].It is known that the solubilities of ILs decrease with the increase in the alkyl chain length of the IL cation [42],suggesting that the use of the IL cation being longer alkyl chain length may generate hydrophobic CF3SO3À-based ILs.Further-more,hydroxyl group has strong ability to form a hydrogen bond; the combination of hydroxyl functionalized cation and CF3SO3Àmay generate a new type of ILs with strong hydrogen-bonding ability. Based on this prediction,in this work,a series of hydrophobic CF3-SO3À-based ILs were synthesized and their extraction ability for CA, FA,p-coumaric acid(p-CA)and sinapic acid(SA)(these4acids are the representatives of hydroxycinnamic acids(Fig.1))was investigated.2.Experimental2.1.MaterialsN-Butylimidazole(99%)and N-benzylimidazole(98%)were obtained from Alfa Chem.,Ltd.(Slough,Berkshire,UK).6-Chloro-1-hexanol(98%),lithium bis(trifluoromethanesulfonyl)imide (LiNTf2,98%),trifluoromethanesulfonic acid(CF3SO3H,99%), sodium tetrafluoroborate(NaBF4,98%)and potassium hexafluo-rophosphate(KPF6,99%)were obtained from Energy Chemical Co.(Shanghai,China).11-Bromo-1-undecanol(P99%)was pur-chased from Fluka(sigma-Aldrich Co.,St.Louis,MO,USA);1-bromobutane(99%),1-bromoheptane(98%),1-bromododecane (98%),CA(99%),FA(99%),p-CA(98%)and SA(98%)were obtained from Aladdin Reagent Co.(Shanghai,China).Chromatographic grade methanol was purchased from Fisher Scientific(Fair Lawn, NJ,USA).Reichardt’s dye(RD,90%)and4-nitroaniline(NA, P99%)were obtained from sigma-Aldrich Co.;N,N-diethyl-4-nitroaniline(DENA,97%)was purchased from Fluorochem Ltd., (Hadfield,UK).Sodium perchlorate monohydrate(NaClO4ÁH2O, 99%)was obtained from Maya Reagent Co.,(Jiaxing,China).The ILs,[C4mim][PF6](99%)and[C6mim][PF6](99%)was obtained from Lanzhou Institute of Chemical Physics of the Chinese Academy of Sciences(Lanzhou,China).The ILs,1-butyl-3-(6-hydroxyhexyl)imidazolium bis(trifluoro methylsulfonyl)imide([C4C6OHim]NTf2),1-butyl-3-(6-hydroxy hexyl)imidazolium hexafluorophosphate([C4C6OHim]PF6),1-butyl-3-heptylimidazolium hexafluorophosphate([C4C7im]PF6), 1-butyl-3-heptylimidazolium tetrafluoroborate([C4C7im]BF4),1-butyl-3-heptylimidazolium bis(trifluoromethylsulfonyl)imide ([C4C7im]NTf2),1-butyl-3-benzylimidazolium bis(trifluoromethyl sulfonyl)imide([C4Bzim]NTf2),1-butyl-3-dodecylimidazolium bis (trifluoromethylsulfonyl)imide([C4C12im]NTf2),1-butyl-3-dodecylimidazolium tetrafluoroborate([C4C12im]BF4),1-butyl-3-dodecylimidazolium hexafluorophosphate([C4C12im]PF6),1-buty l-3-(11-hydroxyundecyl)imidazolium tetrafluoroborate([C4C11-OHim]BF4),1-butyl-3-(11-hydroxyundecyl)imidazolium hexafluo-rophosphate([C4C11OHim]PF6)and1-butyl-3-(11-hydroxyundecyl)imidazolium bis(trifluoromethylsulfonyl)imide ([C4C11OHim]NTf2)were synthesized as described in our previous work[43];the synthetic procedures and characterization of1-bu tyl-3-(6-hydroxyhexyl)imidazolium perchlorate([C4C6OHim] ClO4),1-butyl-3-(6-hydroxyhexyl)imidazolium trifluoromethane-sulfonate([C4C6OHim]CF3SO3),1-butyl-3-heptylimidazolium per-chlorate([C4C7im]ClO4),1-butyl-3-heptylimidazolium trifluoromethanesulfonate([C4C7im]CF3SO3),1-butyl-3-dodecylimidazolium perchlorate([C4C12im]ClO4),1-butyl-3-dodecylimidazolium trifluoromethanesulfonate([C4C12im]CF3SO3), 1-butyl-3-(11-hydroxyundecyl)imidazolium perchlorate([C4C11-OHim]ClO4)and1-butyl-3-(11-hydroxyundecyl)imidazolium tri-fluoromethanesulfonate([C4C11OHim]CF3SO3)were shown in the Supplementary Information(SI).All the other reagents are of ana-lytical grade unless stated.Ultrapure water(18.2M XÁcm)pro-Fig.1.Chemical structures of FA,CA,p-CA,and SA.Y.Fan et al./Separation and Purification Technology179(2017)126–134127duced by an Aquapro purification system(Aquapro International Co.,Ltd.,Dover,USA)was used throughout the experiments.The pH values of the aqueous solutions were controlled by phosphate buffers(0.050mol LÀ1)and measured by a pHS-3B dig-ital pH-meter(Shanghai Leici Instrument Factory,Shanghai, China).2.2.Measurements of organic acidsThe concentrations of CA,FA,p-CA and SA in water phase were measured by a high performance liquid chromatograph(HPLC, 1200model,Agilent Technologies,Santa Clara,CA,USA)equipped with a variable-wavelength detector(VWD)and an autosampler. The separation column was a ZORBAX Eclipse XDB-C18column (4.6mmÂ50mm,1.8l m,Agilent Technologies)and the column temperature was set at303K.The mobile phase was the mixture of methanol and0.10%(V:V)acetic acid aqueous solution(23:77, V:V)with aflow rate of0.60mL minÀ1.The detection wavelength was set at310nm and the injection volume was10l L.2.3.Extraction procedureThe extraction of CA,FA,p-CA and SA was carried out at 298±1K.Generally,0.20mL of a specific IL was mixed with 3.0mL of the aqueous solution of the four acids(1.0Â10À2g LÀ1 for each acid)under stirring for10min which was the minimum time established by the preliminary experiments to achieve extrac-tion equilibrium.After extraction,the IL and water phases were separated by using a centrifuge.The extraction efficiency(E)is cal-culated by the equation:E¼1ÀC w C o wÂ100%ð1Þwhere C o w and C w are the concentrations of an organic acid in aque-ous phase before and after extraction,respectively.The distribution ratio(D)is defined as:D¼C ILC wð2Þwhere C IL and C w are the concentrations of an organic acid in the IL and water phases,respectively.The concentration of a specific organic acid in water phase was measured by the aforementioned HPLC method;the concentration of a specific organic acid in the IL phase was calculated by mass balance.In order to accurately measuring D values,the IL and aqueous phases were mutually sat-urated with each other before extraction to reduce their volume changes.The relationship between E and D can be expressed by the following equation:E¼DDþV wV ILÂ100%ð3Þwhere V IL and V w are the volumes of the IL and water phases, respectively.2.4.Measurements of the hydrophobic parameters of ILsGenerally,the logarithmic value of n-octanol–water partition coefficient(log P ow)is used as a measure of molecular hydropho-bicity.The log P ow values of the ILs used in this work were mea-sured via the method reported in our previous work[43]. Typically,the IL solutions(1.0Â10À4mol LÀ1for each)were pre-pared with water saturated by n-octanol;the n-octanol was also saturated by water before extraction to reduce the volume changes of water and n-octanol phases;10mL of a specific IL solution was mixed with10mL of n-octanol under stirring for30min at 298±1K;phase separation was achieved by centrifugation.The IL concentrations both in the n-octanol and water phases were measured by HPLC method.The chromatographic conditions were as follows:injection volume, 2.0l L;detection wavelength, 220nm;flow rate,0.80mL minÀ1;mobile phase,the mixture of methanol and 2.0Â10À3mol LÀ1of aqueous sodium1-heptanesulfonate solution:95%(V:V)of methanol was adopted for the analysis of the[C4C12im]+-based ILs and75%of methanol was selected for the determination of all the remaining ILs.The P ow value is calculated by the following equation[43]:P ow¼C n-octanolC waterð4Þwhere C n-octanol and C water are the concentrations of a specific IL in the n-octanol and water phases,respectively.2.5.Measurements of the hydrogen-bonding parameters of the ILsThe hydrogen-bonding parameters,a(hydrogen bond donating ability),b(hydrogen bond accepting ability)of the ILs studied in this work were measured by using the three dyes,RD,DENA and NA as probes via the reported method[44].The concentrations of DENA and NA in the ILs were both2.5Â10À5mol LÀ1;the concen-trations of RD in ILs ranged from5.0Â10À4to4.0Â10À3mol LÀ1. The maximum absorption wavelengths(k max)of the three dyes were measured by a TU-1810ultraviolet–visible(UV–Vis)spec-trophotometer(Purkinje General Instrument Co.,Beijing,China). The hydrogen-bonding parameters(a and b)of ILs are calculated by the following equations[44]:mmaxðcmÀ1Þ¼104kðnmÞð5ÞE Tð30Þ¼28;592k maxðnm;RDÞð6Þpü0:314Âð27:52Àm maxðDENAÞÞð7Þa¼0:0649ÂE Tð30ÞÀ2:03À0:72pÃð8Þb¼1:035Âm maxðDENAÞþ2:64Àm maxðNAÞ2:8ð9Þ2.6.Measurements of the solubilities of ILs in waterThe solubilities of ILs in water were measured at298±1K via the reported method[45].Typically,the IL and water phases were vigorously stirred for1h;and then the two phases were separated by centrifugation.The absorbance of the IL-saturated aqueous solutions at220nm was measured by the UV–Vis spectropho-tometer;the concentration(solubility)of a specific IL in water was then calculated by using the Lambert-Beer law.2.7.Determination of FÀin water phaseThe concentration of FÀin water was measured by an ion chro-matograph(IC-2001,Tosoh Corp.,Tokyo,Japan)equipped with a conductivity detector.The chromatographic conditions were as fol-lows:separation column,TSKgel SuperIC-AZ anion exchange col-umn(4.6mmÂ15.0cm,4l m,Tosoh Corp.,Tokyo,Japan); mobile phase,the aqueous solution containing6.3Â10À3mol LÀ1 of NaHCO3and 1.7Â10À3mol LÀ1of Na2CO3;flow rate, 0.6mL minÀ1;injection volume,30l L;detection mode,sup-pressed conductivity.128Y.Fan et al./Separation and Purification Technology179(2017)126–1342.8.Measurements of viscosities of the ILsThe viscosities of ILs were measured by a rotary viscometer (model:NDJ-8S,Changji Geological Instrument Co.,Ltd.,Shanghai,China)at 298±1K.All the above experiments were conducted in triplicate and the data presented in this work are the average values.3.Results and discussionThe ILs,[C 4C 6OHim]BF 4[43]and [C 4C 6OHim]CF 3SO 3(details are shown in the SI)are totally miscible with water and thus they were not used in this work.Additionally,the solubilities of the ILs used in this work in water were measured and the results are listed in Table S1in the SI .3.1.Influence of chemical structures of ILs on the distribution ratio For the sake of convenience of discussion,the ILs except [C 4-Bzim]NTf 2(this IL will be discussed separately below)were divided into four groups:(I)[C 4C 7im]PF 6,[C 4C 7im]BF 4,[C 4C 7im]NTf 2,[C 4C 7im]ClO 4and [C 4C 7im]CF 3SO 3;(II)[C 4C 6OHim]PF 6,[C 4C 6-OHim]NTf 2and [C 4C 6OHim]ClO 4;(III)[C 4C 12im]PF 6,[C 4C 12im]BF 4,[C 4C 12im]ClO 4,[C 4C 12im]NTf 2and [C 4C 12im]CF 3SO 3;(IV)[C 4C 11-OHim]PF 6,[C 4C 11OHim]BF 4,[C 4C 11OHim]ClO 4,[C 4C 11OHim]NTf 2and [C 4C 11OHim]CF 3SO 3.The ILs in the same group have the same cation.The extraction ability (D values)of the 19ILs used in this work for SA is shown in Fig.2.As can be seen,five interesting phe-nomena can be obtained:(I)for the ILs with the same cation,the influence of the IL anion on the extraction ability (D values)forSA follows the trend:PF 6À%NTf 2À<BF 4À%ClO 4À<CF 3SO 3À.Toméet al.suggested that hydrophobicity and hydrogen-bonding ability of the ILs are the main parameters governing the relative affinity of the amino acids with the IL and water phases [46].Therefore,the hydrophobicity (log P ow )and hydrogen-bonding ability of ILs used in this work were determined.It should be noted that Lungwitz et al.suggested that the product of a and b (a b )was an ideal indi-cator of the hydrogen-bonding ability of ILs [38];this strategy was adopted in this work.The correlation between the hydrophobicity and the extraction ability of ILs for the extraction of SA is also shown in Fig.2.The hydrogen-bonding ability of ILs is listed in Table 1.As can be seen from Fig.2,the hydrophobicity of the ILs with the same cation but different anions follows the order:BF 4À<ClO 4À<PF 6À<CF 3SO 3À<NTf 2À(e.g.log P ow ([C 4C 7im]BF 4)<log P ow ([C 4C 7im]ClO 4)<log P ow ([C 4C 7im]PF 6)<log P ow ([C 4C 7im]CF 3SO 3)<log P ow ([C 4C 7im]NTf 2)),which is not consistent with the above mentioned order of the influence of the IL anion on the extraction ability,suggesting that hydrophobicity is not the major driving force underlying the extraction process.As shown in Table 1,the hydrogen-bonding ability of the ILs with the same cation butdifferent anions increases in the order:PF 6À%NTf 2À<BF 4À%ClO 4À<CF 3SO 3À,which is consistent with the above mentioned trend of the influence of the IL anion on the extraction ability,indi-cating that hydrogen-bonding interaction is the major driving force underlying the extraction process.(II)For the dialkylimidazolium-based ILs (ILs in group I and III),the increase in the alkyl chain length of the IL cation results in the decrease in the extraction ability (e.g.D ([C 4C 12im]BF 4<D ([C 4C 7im]BF 4)).This can be explained by the steric hindrance:SA bears large size group (aromatic ring);the increase in the alkyl chain length of the IL cation will hinder the interaction between ILs and SA [46,47].(III)For the hydroxyl functionalized ILs (groups II and IV),the increase in the alkyl chain length of the IL cation improves the extraction ability of the ILs (e.g.D ([C 4C 6OHim]PF 6)<D ([C 4C 11-OHim]PF 6)).As illustrated in Fig.2,the introduction of hydroxylgroup on the IL cation decreases the hydrophobicity (e.g.log P ow ([C 4C 6OHim]PF 6)<log P ow ([C 4C 7im]PF 6));the hydrophobicity of the ILs increases with prolonging the alkyl chain length of the IL cation.Higher hydrophobicity means stronger hydrophobic interaction between ILs and SA,enhancing the extraction ability of ILs accordingly.A long alkyl chain of the IL cation originates steric hindrance,consequently reducing the extraction ability of ILs.That is to say,there is a delicate balance between hydrophobic-ity and steric hindrance.For the hydroxyl functionalized ILs,the influence of hydrophobic interaction is more noticeable than that of steric hindrance.(IV)From the comparison of group I versus group II and group III versus group VI,it can be observed that the incorporation of hydroxyl on the IL cation improves the extrac-tion ability (e.g.D ([C 4C 11OHim]PF 6)>D ([C 4C 12im]PF 6))with the exception of [C 4C 6OHim]ClO 4(its extraction ability for SA is lower than that of [C 4C 7im]ClO 4).Two aspects should be considered to explain this phenomenon:the incorporation of hydroxyl group on the IL cation enhances the hydrogen-bonding strength (e.g.a b ([C 4C 11OHim]PF 6)>a b ([C 4C 12im]PF 6))(Table 1),improving the extraction ability accordingly;on the other hand,[C 4C 6OHim]ClO 4is the most hydrophilic IL (water solubility,65.5g L À1,Table S1in the SI ),which implies that the hydrophobic interactionFig. 2.Correlation of the extraction ability and hydrophobicity of ILs for SA (C SA =1.0Â10À2g L À1,V w :V IL =15:1,pH 2.0).Y.Fan et al./Separation and Purification Technology 179(2017)126–134129between [C 4C 6OHim]ClO 4and SA is rather poor,resulting in the decrease of the extraction ability.(V)Many works have suggested that p –p stacking between ILs and solutes helps improve the extraction ability [40,46,48].However,as shown in Fig.2,[C 4-Bzim]NTf 2,owning stronger p –p stacking due to the introduction of benzyl group on the IL cation,has similar extraction ability to [C 4C 7im]NTf 2,indicating that the role of p –p stacking can be ignored.Additionally,the viscosity (g )of an extractant also influences the extraction efficiency;high viscous extractant is expected to decrease the mass transfer rates [49,50].Therefore,the viscosities of the ILs used in this work were measured.The results listed in Table 1indicate that the NTf 2À-based ILs have the lowest viscosi-ties;however,their extraction ability is lower than that of BF 4À,ClO 4Àand CF 3SO 3À-based ILs and close to that of PF 6À-based ILs (e.g.,g ([C 4C 11OHim]PF 6)>g ([C 4C 11OHim]BF 4)%g ([C 4C 11OHim]ClO 4)>g ([C 4C 11OHim]CF 3SO 3)>g ([C 4C 11OHim]NTf 2);D ([C 4C 11OHim]CF 3SO 3)>D ([C 4C 11OHim]BF 4)%D ([C 4C 11OHim]ClO 4)>D ([C 4C 11OHim]PF 6)%D ([C 4C 11OHim]NTf 2)).This suggests that vis-cosities are not the key parameter affecting the extraction ability of ILs.The extraction behavior of the 19ILs for FA,CA and p -CA is sim-ilar to SA and will not be discussed further here (Figs.S8–S10in the SI ).In view of the fact that [C 4C 11OHim]CF 3SO 3exhibits strongest extraction ability for the four hydroxycinnamic acids,it was then selected in the subsequent studies.3.2.Extraction stiochiometryOn the basis of the characteristics of liquid-liquid extraction,the stoichiometry of the extraction of the four acids from acidic aqueous solution with an IL (taking [C 4C 11OHim]CF 3SO 3for exam-ple)can be expressed by the following equation:OA ða ÞþC 4C 11OHim ½ CF 3SO 3ðÞo !K AOA ÁC 4C 11OHim ½ CF 3SO 3ðÞoð10Þwhere OA,‘‘a”,‘‘o”and K A represent an organic acid,aqueous phase,organic phase (the IL phase)and extraction constant (equilibrium constant),respectively.The extraction constant,K A ,can be calcu-lated as follows:K A ¼OA ÁC 4C 11OHim ½ CF 3SO 3½ o OA ½ a ¼C OA ðIL ÞC OA ða Þ¼Dð11Þthat is to say,K A is equal to D .As mentioned above,the D values of the ILs used in this work for the four acids are illustrated in Figs.2and S8–S10in the SI ,respectively.3.3.Stability of [C 4C 11OHim]CF 3SO 3It is known that PF 6Àand BF 4Àare unstable anions and prone to decomposition with the release of highly corrosive HF,especially in the presence water [24,25].To investigate the stability of [C 4C 11-OHim]CF 3SO 3against hydrolysis,additional experiments were conducted by contacting 0.10g of [C 4C 11OHim]CF 3SO 3with 10mL of water at 298K for 20days.It was found that no F Àwas detected in aqueous phase,suggesting that [C 4C 11OHim]CF 3SO 3is highly stable against hydrolysis.3.4.Thermodynamic analysisAs mentioned above,hydrogen-bonding interaction between ILs and hydroxycinnamic acids is the major driving force underly-ing the extraction process.To further confirm this deduction,ther-modynamic analysis was then carried out.The Gibbs free energy change (D G )of the extraction process can be calculated by the equation [51]:D G ¼ÀRT ln D ð12Þwhere R and T are the gas constant and temperature,respectively.If enthalpy change (D H )and entropy change (D S )keep constant over the studied temperature range;their values can be calculated by using van’t Hoff equation [51]:ln D ¼ÀD H R T þD SRð13ÞThe graphs of ln D versus 1/T for the extraction of the fourhydroxycinnamic acids are shown in Figs.S11–S14in the SI .The resultant thermodynamic parameters (D G ,D H and D S )are listed in Table 2.Negative D G suggests that the extraction of the four hydroxycinnamic acids is a spontaneous process [51,52];D H <0and D S <0imply that hydrogen-bonding interaction is the major driving force underlying the extraction process [51–54].3.5.Influence of pHExperiments indicated that CA and SA are unstable in alkaline media;the influence of pH on the extraction efficiencies of CA and SA were therefore studied in the pH range of 2.0to 7.0.The influence of the pH of aqueous phase on the D values and extrac-tion efficiencies of FA is shown in Fig.3and the influence of pH on the D values and extraction efficiencies of p -CA,CA and SA is shown in Figs.S15–S17in the SI .As shown in these figures,the extraction efficiencies and D values of the four acids keep constant within the pH range of 2.0–4.0and decrease with further increase in pH.It is well known that an organic acid can exist in different forms depending on pH and its dissociation constant (p K a );the p K a values of CA (p K a1=4.38;p K a2=8.58;p K a3=11.50[55]),p -CA (p K a1=4.32;p K a2=8.97[56]),FA (p K a1=4.50;p K a2=8.92[55])and SA (p K a1=4.40;p K a2=9.21[57])have been reported.The four acids mainly exist in neutral forms in the pH range of 2.0–4.0,i.e.the undissociated carboxyl and hydroxyl groups are predominant.It will be expected that strong hydrogen-bonding interaction between ILs and the four acids is formed,resulting in higher extraction efficiencies accordingly.With further increase in pH,the carboxyl and hydroxyl groups of the four acids begin to dissociate,weakening the hydrogen-bonding interaction between ILs and the four acids,leading to the decrease in the extraction efficiencies.Based on these results,pH 4.0was regarded as the optimal pH value for the following experiments.Table 1The hydrogen-bonding parameters and viscosities of the ILs used in this work (average value,n =3).ILab a bViscosity (mPa Ás)[C 4C 7im]PF 60.530.250.13 5.5Â102[C 4C 7im]NTf 20.530.250.13 1.1Â102[C 4C 7im]BF 40.540.470.25 3.5Â102[C 4C 7im]ClO 40.540.420.23 4.8Â102[C 4C 7im]CF 3SO 30.530.570.30 2.7Â102[C 4Bzim]NTf 20.540.240.13 1.5Â102[C 4C 6OHim]PF 60.760.290.228.4Â102[C 4C 6OHim]NTf 20.760.320.24 1.8Â102[C 4C 6OHim]ClO 40.640.500.32 3.6Â102[C 4C 12im]PF 60.520.270.14 1.7Â103[C 4C 12im]NTf 20.510.260.13 2.3Â102[C 4C 12im]BF 40.540.480.26 1.2Â103[C 4C 12im]ClO 40.560.440.25 1.3Â103[C 4C 12im]CF 3SO 30.540.580.31 6.9Â102[C 4C 11OHim]PF 60.640.340.22 1.7Â103[C 4C 11OHim]NTf 20.590.400.24 6.6Â102[C 4C 11OHim]BF 40.660.480.32 1.4Â103[C 4C 11OHim]ClO 40.660.470.31 1.4Â103[C 4C 11OHim]CF 3SO 30.620.590.377.5Â102130Y.Fan et al./Separation and Purification Technology 179(2017)126–134。

响应面法优化马齿苋黄酮超声波提取工艺

响应面法优化马齿苋黄酮超声波提取工艺

响应面法优化马齿苋黄酮超声波提取工艺王波;张晓艳;黄攀;吕德雅;严帆;刘辉【摘要】以野生马齿苋为试验材料,在单因素试验基础上,采用Box-Behnken试验设计和响应面分析法,探讨乙醇体积分数、液料比、提取时间以及提取温度对马齿苋黄酮提取率的影响.结果表明:优化的马齿苋黄酮超声波法提取工艺条件为乙醇体积分数80%、液料比30 : 1(ml/g)、提取时间55.40 min、提取温度64.19 ℃,此条件下马齿苋黄酮理论提取率为1.42%,实际提取率为1.38%.回归模型的预测值与实测值接近,表明响应面法对马齿苋黄酮提取工艺的优化合理可行.%Using Portulace oleracea L.as material,the effects of ethanol volume fraction,ratio of liquid-to-solid,ex-traction time and extraction temperature on the extraction yield of flavonoid were determined through response surface meth-odology based on Box-Behnken experimental design. The results showed that optimum extraction conditions were 80.00%, 30 :1(ml/g),55.40 min and 64.19℃ for ethanol volume fraction,ratio of liquid-to-solid,extraction time and extraction temperature,respectively. Under these conditions,the predicted and actual extraction rates of flavonoid from Portulace oler-acea L. were 1.42% and 1.38%, respectively. The predictive value of the regression model agreed with the experimental value,and the optimized conditions for flavonoid extraction from Portulace oleracea L. were reliable.【期刊名称】《江苏农业学报》【年(卷),期】2018(034)001【总页数】6页(P166-171)【关键词】马齿苋;黄酮;超声波提取;响应面优化【作者】王波;张晓艳;黄攀;吕德雅;严帆;刘辉【作者单位】安徽师范大学环境科学与工程学院,安徽芜湖241002;安徽师范大学环境科学与工程学院,安徽芜湖241002;安徽师范大学环境科学与工程学院,安徽芜湖241002;安徽师范大学环境科学与工程学院,安徽芜湖241002;安徽师范大学环境科学与工程学院,安徽芜湖241002;安徽师范大学环境科学与工程学院,安徽芜湖241002【正文语种】中文【中图分类】TS218马齿苋(Portulace oleracea L.)是马齿苋科马齿苋属一年生肉质草本植物,又名蚂蚁菜、长命菜、瓜子菜、五行草等,在中国南北方均有分布,资源十分丰富[1-3]。

响应面法优化马鞭草中总黄酮闪式提取工艺及其体外抗氧化活性

响应面法优化马鞭草中总黄酮闪式提取工艺及其体外抗氧化活性

响应面法优化马鞭草中总黄酮闪式提取工艺及其体外抗氧化活性张迪【摘要】采用响应面法优化马鞭草中总黄酮的提取工艺.在单因素实验的基础上,以乙醇浓度(A)、料液比(B)、提取时间(C)、提取次数(D)为自变量,总黄酮含量为因变量,运用Box-Behnken设计-响应面优化马鞭草中总黄酮闪式提取工艺.并通过马鞭草总黄酮对DPPH自由基、羟自由基和超氧阴离子自由基的清除作用来评价其抗氧化活性.结果表明:马鞭草中总黄酮提取的最佳工艺条件为乙醇浓度50%,料液比为1∶35 (g/mL),提取时间为1.5 min,提取次数为2次.在此条件下,总黄酮含量达到(8.282±0.003) mg/g,与模型预测值8.280 mg/g相近.重复性试验结果表明,此方法稳定可靠,总黄酮得率高,适于马鞭草中总黄酮的提取.体外抗氧化活性实验表明,当马鞭草中总黄酮浓度为60 μg/mL时,其对DPPH、羟基自由基、超氧阴离子3种自由基清除率分别为74.8%、43.2%、89.5%,表明马鞭草总黄酮具有较强的体外抗氧化活性.【期刊名称】《食品工业科技》【年(卷),期】2019(040)003【总页数】7页(P173-178,184)【关键词】马鞭草;总黄酮;响应面法;抗氧化【作者】张迪【作者单位】南阳医学高等专科学校,河南南阳473061【正文语种】中文【中图分类】TS201.1马鞭草(Verbena officinalis L.)为马鞭草科植物马鞭草的干燥地上部分,马鞭草作为传统中药,收录于《中国药典》之中,具有活血散瘀、解毒、利水消肿、退黄、截疟等功效[1-2],在临床上广泛用于治疗白喉、疟疾等症状。

《中国药典》2015版将马鞭草中齐墩果酸和熊果酸作为马鞭草质量控制的主要指标,但是马鞭草中还存在多种化学成分如:黄酮类、挥发油类、环烯醚萜类、糖类等[3-4]。

这些化学成分也具有显著的活性作用,故亟需对其理化性质及生物活性进行研究分析。

超声辅助双水相提取绞股蓝皂苷工艺及其降糖活性分析

超声辅助双水相提取绞股蓝皂苷工艺及其降糖活性分析

周飙,胡斌,柳鑫,等. 超声辅助双水相提取绞股蓝皂苷工艺及其降糖活性分析[J]. 食品工业科技,2023,44(20):197−205. doi:10.13386/j.issn1002-0306.2022110311ZHOU Biao, HU Bin, LIU Xin, et al. Optimization of Ultrasonic-Assisted Aqueous Two-phase Extraction of Gypenosides and Its Hypoglycemic Activity[J]. Science and Technology of Food Industry, 2023, 44(20): 197−205. (in Chinese with English abstract). doi:10.13386/j.issn1002-0306.2022110311· 工艺技术 ·超声辅助双水相提取绞股蓝皂苷工艺及其降糖活性分析周 飙,胡 斌,柳 鑫,周 蕾*(武汉市第四医院,药剂科,湖北武汉 430034)摘 要:本研究探讨了超声辅助双水相提取绞股蓝皂苷工艺及其降糖活性。

制备6种不同组分的双水相体系,以绞股蓝皂苷得率为指标,筛选得率最高的溶剂体系,通过单因素实验和响应面法考察液料比、超声时间、提取温度,获得最佳提取工艺,并结合主成分分析、分子对接、降糖活性,评价超声辅助双水相提取绞股蓝皂苷的技术优势。

结果表明,选取30%乙醇-20%硫酸铵作为绞股蓝皂苷的提取溶剂,最佳工艺为液料比28:1 mL/g 、超声时间52 min 、提取温度52 ℃。

在此条件下,绞股蓝皂苷得率为7.91%,抑制α-葡萄糖苷酶IC 50为20.2 μg/mL 。

绞股蓝皂苷XLIX 、人参皂苷Rb 3、绞股蓝皂苷A 、绞股蓝皂苷XVII 得率分别为0.83%、0.09%、1.42%、4.04%,与α-葡萄糖苷酶结合能分别为−9.4、−7.7、−7.7、−7.7 kcal/mol 。

咖啡类黑精提取工艺优化及结构表征

咖啡类黑精提取工艺优化及结构表征

王燕华,王冬钰,何泽娟,等. 咖啡类黑精提取工艺优化及结构表征[J]. 食品工业科技,2023,44(19):225−234. doi:10.13386/j.issn1002-0306.2022110097WANG Yanhua, WANG Dongyu, HE Zejuan, et al. Optimization of Extraction Process and Structure Characterization of Coffee Melanoidins[J]. Science and Technology of Food Industry, 2023, 44(19): 225−234. (in Chinese with English abstract). doi:10.13386/j.issn1002-0306.2022110097· 工艺技术 ·咖啡类黑精提取工艺优化及结构表征王燕华1,王冬钰1,何泽娟1,施汤伟1,龚加顺1,2,谭 超1, *(1.云南农业大学食品科学技术学院,云南昆明 650201;2.云南省农业科学院,云南昆明 650201)摘 要:本研究以云南小粒咖啡为研究对象,优化咖啡类黑精提取工艺,利用100、50、30 kDa 的滤膜分级,基于分子形貌、光谱学特性表征不同分子量段的咖啡类黑精结构。

结果表明:咖啡类黑精最佳提取工艺为:料液比1:16(g/mL ),提取温度80 ℃,提取时间60 min 。

凝胶渗透色谱结果表明咖啡类黑精在溶液中呈现紧密球形结构,分子量大小主要为4.56×104和2.94×104 Da ,占比分别为72.5%和27.5%。

X-射线衍射表明咖啡类黑精内部结晶性很弱,属无定形结构。

微观形貌特征分析表明未经分级处理的咖啡类黑精呈表面粗糙且存在孔隙的不规则团聚球形,分级处理后聚合结构消失,呈不规则片状和长条状。

响应面法优化提取紫苏籽饼粕迷迭香酸及其抗氧化能力研究

响应面法优化提取紫苏籽饼粕迷迭香酸及其抗氧化能力研究

响应面法优化提取紫苏籽饼粕迷迭香酸及其抗氧化能力研究闫拯;王乐;袁施彬【摘要】应用超声波辅助(UAE)提取紫苏饼粕迷迭香酸,通过响应面法(RSM)分析数据,优化提取条件;采用DP-PH法、甲基紫法和FRAP法,以抗坏血酸(Vc)为对照,测定迷迭香酸的抗氧化能力.实验结果表明,优化后的响应面提取工艺条件为粒径比60目、料液比1∶10、超声时间71 min及超声温度54℃.在此条件下迷迭香酸得率理论值为0.296%,实测值为0.289%;迷迭香酸抗氧化能力弱于Vc,清除自由基能力强于Vc,对铁离子还原能力弱于Vc.其对铁离子还原能力的FRAP值为703.71 mmol Fe2+/100g,清除DPPH和羟基自由基的IC50值为51μg/mL和561μg/mL.本研究提取方法简单、方便快捷、数据准确,有效提高了紫苏饼粕中迷迭香酸的得率,并且验证紫苏饼粕迷迭香酸具备一定的抗氧化能力,可当做天然抗氧化剂的来源.%Rosmarinic acid is extracted from perilla seed meal with the method of ultrasound-assisted extraction (UAE).The data is analyzed by response surface methodology(RSM) and the extraction conditions are optimized.Its antioxidant ability is determined by DPPH,methyl violet and FRAP,and Vc as control.The results show that the optimum extraction conditions are as follows:particle size 60 mesh,liquid to material ratio 10∶ 1,ultrasonic time 71 min and ultrasonic temperature 54 ℃.Under these conditions,the theoretical yield of rosmarinic acid is 0.296%,and the measured value is 0.289%;its acid antioxidant capacity is weaker than Vc,scavenging free radicals is stronger than Vc,and iron reduction ability is weaker than Vc.The FRAP value of the reduction ability of ferric ion is 703.71 mmol Fe2 +/100g,and the IC50 values of scavenging DPPH andhydroxyl radical are 51 μg/mL and 561 μg/mL respectively.It is concluded that the simplicity,convenience,and accuracy of this extraction method of rosemaric acid help to effectively improve the yield of rosmarinic acid in Perilla Seed Meal.It also proves the possibility of rosmarinic acid from perilla seed meal with certain antioxidant capacity being used as a source of natural antioxidants.【期刊名称】《西华师范大学学报(自然科学版)》【年(卷),期】2017(038)002【总页数】7页(P134-140)【关键词】紫苏;饼粕;迷迭香酸;响应曲面;抗氧化能力【作者】闫拯;王乐;袁施彬【作者单位】西华师范大学生命科学学院,四川南充637009;西华师范大学西南野生动植物资源保护教育部重点实验室,四川南充637009【正文语种】中文【中图分类】TS202.3紫苏(Perilla frutescens (L.) Britt.)为唇形科(Lamiaceae)紫苏属(Perilla Linn.),一年生草本自花授粉植物,在我国有悠久的种植历史,华南、华中、华北、东北、西南以及台湾等地都有栽培和野生种[1-2]。

僵蚕升华物的提取与纯化实验报告 -回复

僵蚕升华物的提取与纯化实验报告 -回复

僵蚕升华物的提取与纯化实验报告-回复"Jiāng cán shēnghuáwùde tíqǔyǔchúnhuàshíyàn bàogào" (Extracting and Purifying Sublimated Materials from Silkworm Cocoons: Experimental Report)Abstract:The purpose of this experiment is to extract and purify sublimated materials from silkworm cocoons, which have potential applications in various industries. By following a step-by-step procedure, we successfully obtained pure sublimated materials and characterized their properties. This report provides a comprehensive analysis of the experiment, including the materials and methods used, results obtained, and future applications of the obtained sublimated materials.Introduction:Sublimation is the process of converting a solid directly into a gas without going through the liquid phase. Silkworm cocoons are known to contain sublimated materials that can be further extracted and purified for various purposes such as pharmaceuticals, cosmetics, and industrial applications. This experiment aims to extract and purify these sublimated materialsfrom silkworm cocoons through a series of steps.Materials and Methods:1. Silkworm cocoons: Collect silkworm cocoons from a silkworm farm or purchase them from a supplier.2. Mortar and pestle: Crush the silkworm cocoons into a fine powder.3. Solvent: Choose an appropriate solvent, such as ethanol or acetone, for the extraction process.4. Extraction apparatus: Set up an extraction apparatus, consisting of a heating mantle, round-bottom flask, condenser, and collection flask.5. Distillation apparatus: Prepare a distillation apparatus, includinga round-bottom flask, condenser, and collection flask.6. Filtration: Filter the extracted solution to remove any impurities.7. Purification: Purify the filtered solution through the distillation process.8. Characterization: Analyze the purified sublimated materials using techniques such as gas chromatography or mass spectrometry.Results:The experiment yielded a clear, yellowish solution after crushingand extracting the silkworm cocoons. The extracted solution was then subjected to distillation, resulting in the collection of purified sublimated materials. Gas chromatography analysis revealed the presence of various compounds, including silk proteins, amino acids, and lipids. The purified sublimated materials exhibited high purity and showed promising properties for further applications.Discussion:The successful extraction and purification of sublimated materials from silkworm cocoons highlight the potential of these materials in various industries. Silk proteins have excellent biocompatibility and biodegradability, making them ideal for applications in drug delivery systems and tissue engineering. Amino acids found in the sublimated materials have potential uses in the cosmetic industry due to their moisturizing and anti-aging properties. Lipids present in the purified sublimated materials can be further processed into biofuels or utilized in the production of cosmetic creams.Conclusion:In conclusion, this experiment demonstrated the successful extraction and purification of sublimated materials from silkworm cocoons. The obtained sublimated materials showed promisingproperties for applications in the pharmaceutical, cosmetic, and industrial sectors. Further research and optimization of the extraction and purification processes can lead to enhanced yields and increased purity of these valuable materials. The findings of this study contribute to the utilization of silkworm cocoons in a sustainable and economically viable manner.。

超高压辅助胶束法提取落叶松中二氢槲皮素的工艺优化

超高压辅助胶束法提取落叶松中二氢槲皮素的工艺优化

杨帆,霍志伟,朱雯,等. 超高压辅助胶束法提取落叶松中二氢槲皮素的工艺优化[J]. 食品工业科技,2023,44(23):175−183. doi:10.13386/j.issn1002-0306.2023020026YANG Fan, HUO Zhiwei, ZHU Wen, et al. Optimization of Ultrahigh Pressure Assisted Micellar Extraction of Taxifolin from Larch[J]. Science and Technology of Food Industry, 2023, 44(23): 175−183. (in Chinese with English abstract). doi:10.13386/j.issn1002-0306.2023020026· 工艺技术 ·超高压辅助胶束法提取落叶松中二氢槲皮素的工艺优化杨 帆,霍志伟,朱 雯,赵修华*(东北林业大学化学化工与资源利用学院,黑龙江哈尔滨 150040)摘 要:为简化二氢槲皮素提取工艺,降低能耗与成本,提高提取效率,促进二氢槲皮素的综合应用,本研究采用黑龙江省的兴安落叶松为原料,运用超高压辅助胶束提取技术提取落叶松中二氢槲皮素,测定落叶松树根、树干等不同部位的二氢槲皮素总含量。

以此总含量为基础,对提取胶束进行筛选,采用响应面试验对提取工艺进行优化,考察了料液比、提取压力、提取次数及胶束浓度4种不同因素对二氢槲皮素提取率的影响,并与微波提取、超声提取、回流提取等不同提取工艺进行能耗与CO 2排放比较。

结果表明,最终确定提取胶束为茶皂素,最佳提取工艺条件为:茶皂素浓度8%,料液比1:11.5,提取压力157 MPa ,提取次数3次,保压时间5 min ,在此最佳条件下重复进行3次实验,二氢槲皮素实际提取率可达84.35%±1.20%,与预测值84.98%基本一致。

响应面法优化芦荟中抗氧化活性成分的提取工艺_唐远谋

响应面法优化芦荟中抗氧化活性成分的提取工艺_唐远谋

第9卷第1期2011年1月生 物 加 工 过 程Ch i nese Journa l o f B ioprocess Eng i neer i ng V o.l 9N o .1Jan .2011do:i 10.3969/.j issn .1672-3678.2011.01.006收稿日期:2010-07-14作者简介:唐远谋(1986 ),男,四川南充人,硕士研究生,研究方向:食品营养与安全;焦士蓉(联系人),副教授,硕士生导师,E-m ai:lj s -rong2004@163.co m响应面法优化芦荟中抗氧化活性成分的提取工艺唐远谋1,焦士蓉1,冷 鹂2,唐鹏程1,刘 佳1,冯 慧1(1.西华大学生物工程学院,成都610039;2.四川大学生命科学学院,成都610064)摘 要:对芦荟中抗氧化活性物质提取工艺及其成分进行研究,通过单因素实验和响应面优化,以提取物对DPPH 自由基的清除率为抗氧化的考察指标,得到芦荟中抗氧化活性成分的提取工艺条件:提取温度29 、料液比(g /mL)1 33、提取时间107s 、微波功率500W,微波辅助水提,此条件下得到的提取物对DPPH 自由基的清除率达91 414%。

提取物活性成分分析表明:提取物中芦荟甙含量为1 5m g /g 、黄酮为1 13mg /g 、多酚为4 33m g /g 、多糖为126 36mg /g 。

关键词:芦荟;抗氧化物质;DPPH 自由基;提取;响应曲面法中图分类号:TS201.1 文献标志码:A 文章编号:1672-3678(2011)01-0024-05Opti m izati on of process para m eters of extraction antioxi dantsfro m A loe usi ng response surface m ethodol ogyTANG Yuan m ou 1,JI A O Sh irong 1,LENG L i 2,TANG Pengcheng 1,LI U Jia 1,FENG Hu i1(1.Schoo l o f B i oeng i neer i ng,X i hua U niversity ,Chengdu 610039,China ;2.Schoo l o f L ife Sc i ences ,Sichuan U ni v ers it y ,Chengdu 610064,Chi na)Abst ract :The process para m eters for extraction o f antiox i d ants fro m Aloe w ere opti m ized and the co m po -nents w ere analyzed .The opti m al process conditi o ns w ere attained by sing le factor m ethod and response surface m e t h odogy .Anti o x idant ab ilicy w as evalvated on the scaveng ing rate o fDPP H free radica.l M icro -w ave assisted ex traction(MAE )by w ater w as chosed and t h e solid -li q u i d ratio w as 1 33,m icro w ave po w -er w as 500W at 29 for 107s .Under t h ese conditi o ns ,the re m ova l rate of DPP H w as 91 414%.The resu lts o f co m ponent analysis for antiox idants show ed that the y ie l d of a l o in ,flavono i d s ,po l y pheno ls ,and po l y sacchari d e w ere 1 5m g /g ,1 13m g /g ,4 33m g /g ,and 126 36m g /g ,respectively .K ey w ords :A loe ;anti o x i d ants ;DPP H free rad ica;l extracti o n ;response surface m ethod 芦荟系百合科(L iliaceae )芦荟属(A loe )多年生的常绿、肉质草本植物,原产于非洲[1]。

正交提取法优选刺头复叶耳蕨总黄酮的提取工艺

正交提取法优选刺头复叶耳蕨总黄酮的提取工艺

正交提取法优选刺头复叶耳蕨总黄酮的提取工艺李辉敏【期刊名称】《九江学院学报(自然科学版)》【年(卷),期】2015(000)003【摘要】Objective To study the optimum ultrasonic extraction process for total flavonoids from Arachniodes exilis ching. Method With total flavonoids content as index,the extraction of total flavonoids from Arachniodes exilis ch-ing by orthogonal experiment in the optimum ultrasonic extraction process was optimized. Result The optimum ultrasonic extraction process was using 60% ethanol,1:20 solid - liquid ratio,ultrasonic extraction 30 min with three times. Under these conditions,the yield of total flavonoid extract were 16. 18 mg/ g(total flavonoid/ crude drug). Conclusion The optimized ultrasonic extraction process was reasonable and feasible with high yield.%目的:研究超声波提取法从刺头复叶耳蕨中提取总黄酮的最佳工艺。

方法以总黄酮提取率为评价指标,采用单因素试验及正交试验对超声波提取法的过程参数进行优化。

结果所得最佳提取工艺:溶剂为60%乙醇,料液比为1∶20,超声波辅助提取3次,每次提取30 min,总黄酮的提取率可达到16.18 mg / g(总黄酮量/生药量)。

响应面法优化五味子中五味子醇甲超声提取

响应面法优化五味子中五味子醇甲超声提取

响应面法优化五味子中五味子醇甲超声提取王磊【摘要】The extraction techniques of Schisandrin from Schisandra chinensis(Turcz.) Baill was optimized by response surface methodology.Solid-liquid ratio,ethanol concentration,and extraction ultrasonic power as the response factors,extraction rate of Schisandrin as response value,and response surface analysis implemented by three factors and five levels,response surface model was established,and the optimum technological conditions were obtained.The optimum technological conditions of extracting Schisandrin from Schisandra chinensis(Turcz.) Baill by response surface methodology were that ethanol concentration was 90.06% and extraction ultrasonic power was 401.56 W and solid-liquid ratio was 1:9.99.%利用响应面分析法优化北五味子醇甲的提取工艺,以乙醇浓度、料液比及超声功率为响应因素,五味子醇甲提取率为响应值,实施3因素5水平的响应面分析,建立响应面模型,并得出最佳工艺条件。

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Improved Skeleton Extraction and Surface Generationfor Sketch-based ModelingFlorian Levet∗Xavier Granier†IPARLA project(INRIA futurs-LaBRI),UMR5800,Universite Bordeaux1351,cours de la Libration33405Talence,FranceFigure1:Surface Generation(from left to right):sketched silhouette,extracted skeleton and internal edges,sketched profile curve and resulting model.A BSTRACTFor the generation of freeform models,sketching interfaces haveraised an increasing interest due to their intuitive approach.It isnow possible to infer a3D model directly from a sketched curved.Unfortunately,a limit of current systems is the poor quality of theskeleton automatically extracted from this silhouette,leading to lowquality meshes for the resulting objects.In this paper,we present new solutions that improve the surfacegeneration for sketch-based modeling systems.First,we propose anew algorithm that extracts a smoother skeleton compared to pre-vious approaches.Then,we present a new sampling scheme forthe creation of good-quality3D mesh.Finally,we propose to usea profile curve composed of disconnected components in order tocreate models which genus is greater than0.CR Categories:I.3.5[Computer Graphics]:Computational Ge-ometry and Object Modeling—Modeling packages;I.3.5[Com-puter Graphics]:Computational Geometry and Object Modeling—Curve,surface,solid,and object representations;Keywords:Modeling,FreeForm Surfaces,Sketching,ImplicitSurface1I NTRODUCTIONDue to the large number of tools,the interface of current3D mod-elers are extremely complex and intimidating for non-expert users.Creating a prototype of a3D model can thus become a slow andpainful task.So,in order to provide simpler interfaces,new ap-∗levet@labri.fr†granier@labri.frproaches for3D modeling have been developed,based on the hu-man ability to quickly draw a global overview of an object.Theseapproaches are commonly referred as3D Sketching.Their principleis to infer the shape of a3D model based on sketched2D curves.Onthis model,users can add details thanks to different editing opera-tions(cutting,extrusion,etc,.),all based on sketching interaction.Since all these systems use a drawing metaphor,they can be easilyadopted even by non-expert users.From thefirst freeform modeler based on sketching[10],manyworks have been published that try to improve the surface genera-tion[11,4,8,20,19,7]and the editing operations[18,20,7,14].Among all the editing operations,changing the profile curve[20,7,14]allows an efficient modification of the local or global shape,and the generation of more complex models in few sketches.In this paper,we introduce three main contributions.(i)Thefirstone is a new solution for the skeleton extraction from a silhouettecurve.This skeleton,computed thanks to a2D variational implicitsurface[22]that approximates the silhouette curve,is smootherthan previous algorithms(see Section4).(ii)The second contri-bution is a new approach for inferring the3D volume based on thisskeleton.Its main goal is to provide a better quality mesh withoutinherent artefacts that occur on mesh-based freefrom modeling(seeSection5).(iii)Finally,we propose a solution to generate a modelwith genus greater than0based on more complex profile curves.2P REVIOUS WORKTeddy[10]is the precursor system for the creation of3D freeformmodels by using gestures and curves.In order to infer a3D modelfrom a silhouette,this curve is sampled and the resulting samplesare triangulated with a Constrained Delaunay Triangulation.Basedon this triangulation,a skeleton is extracted.The elevation is com-puted on each vertex of this skeleton based on the average distanceto the nearest silhouette samples.This skeleton extraction heavilydepends on the initial triangulation,and is prone to several arte-facts(see Figure2),leading to a low quality mesh[9].In order(a)(b)Figure2:Limitations of the Teddy approach:(a)the skeleton ex-tracted from the CDT(Constrained Delaunay Traingulation)has some discontinuities and,(b)the sampling of the internal edges leads to very tiny and uneven triangles.to improve the quality of the skeleton,some vertices can be re-moved[20],but the resulting curve still depend on the triangulation and thus on the curve sampling process.Despite these limitations,the algorithm developped in Teddy is used in many related publications[18,4,8,24,20,3,14],mainly due to its simplicity and its versatility.As an example,Owada et al.[18]extend it to voxel-based volume generation.Some other works[4,8,20,24,3]used variational implicit surfaces in order to overcome the problem of mesh quality.By using a simplified skeleton combined with the blending properties of the implicit sur-faces,they were able to improved the model quality.Unfortunately, global editing of the geometry is very expensive since the whole implicit model needs to be reconstructed and repolygonized before visualization.Among all the previous solutions,only profile-based ones[20, 7,14]enable the creation of models that are not limited to blobby shapes.Nevertheless,all of them have some specific limitations and strongly rely on the skeleton quality.Because of the underlying sur-face representation(a polynomial-weighted convolution surface), the definition of the profile curve in the ConvMo[20]environment is limited to polar coordinates.The segment-based skeleton is im-proved by removing some vertices,but it still depends on the initial sampling of the silhouette.In our previous work[14],we have pre-sented a system that can create genus1models.But the resulting mesh relies even more on the initial quality of the skeleton.Cherlin et al.[7]do not use a skeleton,but an interpolating parametric sur-face in order to create models that are not limited to blobby objects. Unfortunately,because they do not extract a skeleton,the resulting models are limited to a grid topology and thus can not have junc-tions.Alexe et al.[2]used an image processing technique for the cre-ation of the skeleton.Thus,from the silhouette curve and a distance image,they can extract a skeleton that do not depend on the initial sampling.This skeleton is composed of segments and polygons. The reconstructed surface is thusflatter in regions where the skele-ton is a polygon.However,this algorithm is not well adapted to profile edition that requires curve or segment-based skeletons. Numerous methods have been proposed to extract the skeleton of a2D shape.They can be classified in two main families:dis-crete methods and continuous methods.Continuous methods are generally based on the V oronoi graph of a point set located on the object boundary[5,6,17].The dual of the V oronoi diagram,the Delaunay triangulation has also been used extensively[1,23]as in Teddy[10].Both approaches preserve topology but,unfortunately, the techniques used to prune faces and edges which correspond to small perturbations of the boundary are mostly based on heuristics.The discrete methods work directly on binary images.For in-stance,methods based on thinning[13,15,12,16]attempt to create a skeleton which preserves the shape topology thanks to the def-inition of some erosion rules.However,these methods are quite sensitive to Euclidean transformations and,besides,they usually yield un-wanted edges.Some sketching systems[19,7]do not use a skeleton to inflate the object volume.Karpenko et al.[11]inflate the object volume by elevating the silhouette gravity center.Some problems may occur when the gravity center is not inside the object silhouette.Schmidt et al[19]used a2D variational implicit surface as an approximation of the silhouette curve.Then,this2Dfield is swept along an infinite 3D axis and bounded.Thanks to this technique,they can create blobby objects,sweep surfaces and surfaces of revolution.3M OTIVATIONThe more versatile solution to generate a3D surface from a2D sil-houette curve still seems to be the algorithm developed in Teddy. But,as said before,this algorithm has some strong limitations. First,the use of a Constrained Delaunay Triangulation(CDT)com-puted from the silhouette curve,leads to the creation of a skeleton with a lot of local oscillations as can be seen in Figure2(a),even in very simple cases.This results in a3D object with a lot of height variations along the skeleton.These variations are propagated on thefinal mesh.While they are less visible with a classical circular profile curve,these artefacts are increased with a freeform profile curve.Besides,even with an improved skeleton[20],different sam-plings of the silhouette lead to different triangulations and thus,to different skeletons and resulting meshes.The second problem occurs for the mesh-based solution and de-pends on the sampling along the internal edges(an internal edge is an edge that connects a silhouette point and a skeleton point).Once elevated,these samples will result in thefinal vertices of the mesh. Since these internal edges are based on the triangulation,more than one internal edge can end on one silhouette point(see Figure2(a)). As can be seen in Figure2(b),this leads to the creation of very tiny and uneven triangles near these silhouette samples.The low quality of the mesh can create some artefacts during the editing operations. In order to improve the quality of the inferred mesh,we have identified two desirable properties for the skeleton and the internal edges:1.the skeleton should be smooth to limit the local variations,2.each silhouette point should be connected to only one internaledge.(a)(b)Figure3:(a)Gradientfield of an implicit surface(from[26]).(b) Silhouette points used to reconstruct the2D variational implicit sur-face.(a)(b)Figure4:(a)Variation of the reconstructed implicit function with some silhouette samples.(b)These samples have moved according to the gradientfield and converged to the vanishing points,corre-sponding to the seeds of our skeleton.To fulfil these properties,we present a two-fold alternative tech-nique compared to existing works.First,in Section4,we propose to compute a smooth skeleton by using a2D variational implicit surface.Then,in Section5,we present a new sampling technique which ensures that only one internal edge corresponds to a silhou-ette point.4C REATION OF THE SKELETONSimilarly to the work of Zonenschein et al.[25]on texturing of im-plicit surfaces,the basic idea of our technique is to use the gradient of a2D variational implicit surface as a forcefield(see Figure3(a)). Thanks to this forcefield,the seed points(we will simply call them seeds)of the skeleton are computed using a two-steps process.4.1Finding the skeleton seedsFirst,a2D variational implicit surface[22]is used as an approx-imation of the silhouette curve sketched by the user.As can be seen in Figure4,the implicit function has some local minima.The corresponding points are called vanishing points(points where the gradient of the implicit function is null)and they represent the seeds of our skeleton.In order tofind the position of the seeds,the gradient of the im-plicit surface is used as a forcefield.A gradient descent is applied on some silhouette samples(see Figure4(a))until their convergence to the vanishing points(as shown in Figure4(b)).In the Figure4, the silhouette has four branches,resulting infive skeleton seeds. This provides us a good representation of the silhouette topology.4.2Neighboring relations of the seedsIn order to create the full skeleton,the seeds have to be con-nected.For this purpose,we compute their neighboring relation-ship.Thanks to the gradient descent,each seed can be associated with the set of its original silhouette samples(samples that have converged to this seed).If two adjacent silhouette samples do not converge to the same seed,the two corresponding seeds are neigh-bors.The neighboring relations between the seeds computed in Figure5correspond to the four branches of the original curve.4.3Creation of new skeleton pointsIn order to create the full skeleton,the curve connecting two neigh-bor seeds has to follow the line of local minimum of the implicit function.An approximation of this curve will be computedby(a)(b)Figure5:(a)Gathering behavior of the silhouette samples:their color is the same that their corresponding seed.(b)Neighboring relations between the seeds.a uniform sampling in-between two connected seeds.The dis-tance between two consecutive skeleton points is evaluated to be d=|r i j|/∆,where r i j is the vector between the two neighboring seeds i and j and∆the desired number of points.For a faster creation of these skeleton points,the process is only based on the evaluation of the implicit function,and the search of a local minimum.In order tofind this minimum,a set of sample points on a circular section are computed in the direction of the next seed,with d as radius and the current seed as its center(Figure6(a)). On the circular section,the position with the minimal value of the implicit function is added as a new point.This process is repeated on the newly added point(Figure6(b))until the distance between the newly inserted point and the second seed is lower than the re-quired distance.This sampling is repeated for all the neighboring relations of the seeds.Since the resulting points follow the local minimum of the implicit function,the skeleton inherits its smooth-ness from the implicit function(as shown in Figure16).5I NFERRING THE VOLUME OF THE OBJECTNow that a smooth skeleton has been extracted from the silhouette curve,the next step of the process is to infer the volume of the object.For afinal higher quality mesh,our system introduces a new creation and sampling of internal edges.5.1Relations between silhouette samples and skeleton points The skeleton seeds(see Section4)are computed from a set of sil-houette samples.These samples are in fact a small subset ofthe(a)(b)Figure6:Creation of new skeleton points.The local minimum of the implicit function is the green dotted line;green points are the added skeleton points while violet points are the non-local minimums of the implicit function evaluation.(a)Starting from thefirst seed,a new skeleton point is added(corresponding to a local minimum).(b)The new point becomes the new starting point.(a)(b)Figure 7:(a)Connecting relations between skeleton points and sil-houette samples.(b)Determination of the S-set of a given skeleton point.complete sampling of the profile curve,since for finding the van-ishing points,only a coarse approximation of the curve is required (in theory,a minimum of one silhouette sample per seed).On the contrary,the creation of the internal edges is facilitated if there are more silhouette samples than skeleton points.Discarding useless samples is easier than adding new points in under-sampled region of the silhouette curve.For the following algorithm,the whole set of silhouette samples is used.The first step of the process is to gather,for each skeleton point,the closest silhouette samples.Based on these connecting sets,the final internal edges are computed based on the following three prop-erties:•There is one internal edge at most for each silhouette sam-ple.This property removes the meshing problem shown in Figure 2(b).•From each extremal skeleton point (point connected to only one neighbor),internal edges are built to link all the silhouette samples which have this point as closer skeleton point (see the green points in Figure 7(a)).The resulting triangle fans accurately represent extremal sections of the silhouette.•From the other skeleton points connected to n other neighbor-ing points (n >1),n internal edges are issued to n silhouette samples that have to be non-adjacent (cf.Figure 7(a)).Based on the connecting sets and these defined properties,the internal edges can be created.For the extremal points,a subset of connected silhouette samples is selected in order to create the triangle fan.For all the other skeleton points,the process is the same.Depending on the number n of neighbor points,its connect silhouette samples are divided in n non-adjacent sets that we call S-sets (n =2in Figure7(b)).(a)(b)Figure 8:(a)Creation of an internal edge for an odd number of samples in the S-set.The blue sample is chosen while the green samples are discarded.(b)If an S-set is empty,a new sample is added between the two silhouette samples of the two closest internal edges.Then,an internal edge is created between this sample and S i .5.2Creation of the internaledges(a)(b)Figure 9:Creation of an internal edge for an even number of samples in the S-set.(a)A new sample is created between the two middle samples of the S-set.(b)This sample is projected on the surface and an internal edge is created between this sample and the skeleton point.We can see the S-sets of a skeleton point as the different sections of silhouette that are controlled by its position.For the creation of an internal edge,the best sample of the S-set is thus the middle of each section.If the number of samples of an S-set is odd,an internal edge is created between the middle sample and the skeleton point (see Figure 8(a))and all the other S-set samples are then discarded.On the contrary,if the number is even,a new silhouette sample is added between the two middle samples and projected onto the implicit sur-face (see Figure 9(a)).An internal edge is created with the skeleton point and all the other S-set samples are discarded (see Figure 9(b)).At the end of the algorithm,some internal edges can be missing (see Figure 8(b)).This corresponds to empty S-sets due to under-sampled region.In order to create a missing internal edge,the sys-tem gathers the two closer internal edges and creates a new sample on the curve between their two corresponding silhouette samples.This new sample is then connected to the current skeleton point.The result of this complete process is a set of internal edges that correspond to the desirable properties defined in Section 5.1(see Figure 10)and,thus,that will lead to good quality 3D meshes.5.3Creation of genus 1+models with profile curveUsing profile curves in order to edit locally or globally the freefrom shape [20,7,14]enables more complex models in a few strokes,but this extension to non-convex curves needs a more precise skeleton,as noted in [20].We can use such an approach with our smooth skeleton and our internal edges extraction:the results are improved,as shown in the comparison between our system (Figure13(a-c))(a)(b)Figure 10:Examples of the internal edges creation for two different silhouette curves.(a)(b)(c)Figure 11:Creation of a genus 1+model.(c)The profile curve is composed of three disconnected components.(a)-(b)The resulting 3D object.and our previous work [14](Figure 13(b-d)).For this model,we have sketched rectangular silhouette and profile curves.Our previous system [14]is limited to genus 1models.We in-troduce here how to generate models with larger genus (genus >1).The user is now not limited to only one profile curve.He can sketch several components (as shown Figure 11(c))before the profile mod-ification is applied on the 3D model.Then,for each internal edge,each disconnected component of the profile curve is sampled,and these samples are reprojected along each internal edge (for a more precise explanation on how the resulting mesh is reconstructed with respect to the profile curve sketched by the user please refer to [14]).The different components appear in the final model,resulting in genus 1+solutions,as shown in Figure 11.6R ESULTS AND DISCUSSIONOne of the main advantages of our approach is a higher quality of the resulting skeleton.Figure 12shows a comparison between our skeleton extraction and the one from Teddy [10].As explained in Section 4,the use of an implicit function leads to the reconstruction of a smoother skeleton without the un-wanted local oscillations (see Figure 12(a-c)).For instance,the Teddy algorithm always extracts a skeleton composed of connected segments even for a near-circular silhouette curves (see Figure 13(b)).The final model will thus not be similar to a sphere.Our algorithm extracts a skeleton composed of a unique point (see Figure 12(b)and Figure 1).The resulting internal edges have a much better quality (see Figure 1)and the inflated 3D model will have less rendering artefacts.Additional skeletons extracted using our technique can be seen in Figure 16.Note that each skeleton is a good approximation of the silhouette topology.As said previously,a smooth skeleton is needed when using profile editing operations.Indeed,skeleton discontinuities lead to height differences in the vertices of the final mesh.Figure 13shows some comparisons between our system (Figure 13(a-c))and our previous one [14]one (Figure 13(b-d))for two different mod-els.For each model,the same silhouette and profile curves were used.Because we have a smoother skeleton and a better sampling,the models reconstructed with our system are smoother and do not present the height differences on the borders of the models.By sketching profile curves with disconnected components,our system allows the users to generate models with genus greaterthan(a)(b)(c)(d)Figure 12:Comparison between the skeleton of Teddy (b)-(d)and ours (a)-(c).Thanks to implicit curve our algorithm manages to create a good skeleton (one point)for circular silhouette curves.Be-sides,for more complex silhouette curves,the skeleton extracted by our technique is smoother.1(see Figure 1and Figure 11).For example,we have created the GI logo (see Figure 14).It was modeled with 3different objects (the profile curves used for each object are shown)within a total of six curves (2for each object).Because of the use of a profile with disconnected components and internal holes,the genus of the letter G is 4(please note that no parametrization was needed,the user only sketched the silhouette of the letter G and the two components of the corresponding profile curve).Besides,unlike most existing systems,our system creates good-quality models when used with non-circular profile curves (see Figure 1,11and 14).The main limitation of our current technique is the determina-tion of the vanishing points.Indeed,they are only dependant of the definition of the implicit function.For instance,if the user draws a silhouette curve with a large enough zig-zag then some vanish-ing points will correspond to this zig-zag.The problem is that we can not control the apparition of these vanishing points.Besides,in some cases,the user may want to have vanishing points correspond-ing to this zig-zag,but in other cases,he may not want to.So,we think that the best solution is to have a semi-automatic generation of the skeleton,the user having the possibility to edit the vanishing points (by discarding some vanishing points,adding news points or moving the existing ones).7C ONCLUSIONIn this paper,we have presented new techniques in order to improve the quality of the models generated using sketch-based freeform modeling systems.The silhouette curve drawn by the user is first approximated by a 2D variational implicit function.From this vari-ational approximation,a skeleton is extracted that inherits from the implicit function its global smoothness.We have also introduced a new scheme to create the set of internal edges which aim is to limit the creation of tiny and uneven triangles.Indeed,better internal(a)(c)(b)(d)Figure13:Comparison between two models generated by our cur-rent system(a)-(c)and our previous one(b)-(d).For each object,the same silhouette and profile curves were used.Because of oursmoother skeleton,models generated with our system do not havethe classical rendering artefacts generated by a skeleton with discon-tinuities.edges lead to the creation of better meshes for thefinal object.Fi-nally,we have presented sampling process in order to create modelswith genus greater than0,based on the sketch of profile curves withholes and disconnected components.After focusing on the improvement of the surface construction,we are now investigating new interactions for sketch-based mod-eling systems.Borrowing some elements from[21],our currentdirection is the integration of different drawing plans on the objectview.We believe that offering the possibility to modify differentviews of the same object can lead to the construction of complexand interesting models.One other direction,is to develop differ-ent editing operations based on the properties of our reconstructedmesh.AcknowledgmentsWe wish to thank Christophe Schlick and the anonymous reviewersfor their helpful remarks and corrections.R EFERENCES[1]M.Af,O.Ubler,R.Kikinis,M.Shenton,and G.Ekely.Character-ization and recognition of2d organ shape in medical image analysisusing skeletonization.In In Proc.Workshop on Mathematical Meth-ods in Biomedical Image Analysis(MMBIA),pages139–150,1996.[2] A.Alexe,L.Barthe,M.P.Cani,and 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Levet,Xavier Granier,and Christophe Schlick.3d sketchingwith profile curves.In International Symposium on Smart Graphics,2006.[15]Antoine Manzanera,Thierry M.Bernard,Francoise J.Preteux,andBernard Longuet.Medial faces from a concise3d thinning algorithm.In ICCV(1),pages337–343,1999.[16]Virginie Marion-Poty and Serge Miguet.A new2-d and3-d thinningalgorithm based on successive border generations.In4th DiscreteGeometry for Computer Imagery,pages195–206,1194.[17]R.L.Ogniewicz and O.K¨u bler.Hierarchic Voronoi skeletons.PatternRecognition,28(3):343–359,1995.[18]S.Owada,F.Nielsen,K.Nakazawa,and T.Igarashi.A SketchingInterface for Modeling the Internal Structures of3D Shapes.In Proc.Smart Graphics,pages49–57.Springer-Verlag,July2003.[19]R.Schmidt,B.Wyvill,M.C.Sousa,and J.A.Jorge.ShapeShop:。

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