HPLC Determination of Vitexin and Isovitexin from Crotalaria Sessiliflora L. with Response Surface Method to the Optimization of Conditions of Microwave Assisted Sample Extraction
摘 要
应用响应面法优化了乙醇微波辅助萃取农吉利中牡荆素和异牡荆素的条件,用高效液相色谱法测定提取液中牡荆素和异牡荆素的含量。用单因素试验选取了萃取温度、液料比及萃取时间等3项条件,并在此基础上,用中心组合试验设计,采用三因素三水平数学模型和响应面法分析进行优化,确定了最优提取条件为:① 萃取温度152 ℃;② 液料比为44∶1;③ 萃取时间6.6 min。在此条件下牡荆素和异牡荆素的提取率分别为253.3,236.9 μg·g-1,与理论值相近。样品加标回收率分别在97.0%~104%和96.0%~102%之间。
Abstract
The conditions for microwave assisted extraction of vitexin and isovitexin in Crotalaria sessiliflora L. with ethanol were optimized by applying the response surface method. Contents of vitexin and isovitexin in the extracts were determined by HPLC. Single factor testings were performed to select the conditions of extraction temperature, volume (mL) to mass (g) ratio of extracting solvent (C2H5OH) to sample and extraction time; and the conditions were optimized further by applying the central composite design principle at the mode of 3-factors and 3-levels, and the response surface analysis. The optimum extraction conditions found finally were as follow: ① extraction temperature of 152 ℃; ② ratio of C2H5OH (mL) to sample (g) of 44∶1; ③ extraction time of 6.6 min. Rate of extraction obtained under the optimum conditions attained to 253.3 μg·g-1 (for vitexin) and 236.9 μg·g-1 (for isovitexin), which were very close to the theoretical values. Values of recovery obtained by standard addition method were in the ranges of 97.0%-104% for vitexin and 96.0%-102% for isovitexin.
中图分类号 O652.63
所属栏目 试验与研究
基金项目 广州市科技支撑计划项目(2008Z1-E301);广东药学院师资队伍建设基金项目(52104109)
收稿日期 2012/2/13
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备注王李平(1985-),男,安徽安庆人,硕士研究生,主要从事药物的提取分离及分析研究。
引用该论文: WANG Li-ping,LIU Xiao-qin,FAN Hua-jun,SHE Xu-hui,XIAO Xue-xia,HUANG Xiao-wen. HPLC Determination of Vitexin and Isovitexin from Crotalaria Sessiliflora L. with Response Surface Method to the Optimization of Conditions of Microwave Assisted Sample Extraction[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2013, 49(2): 129~133
王李平,刘小琴,范华均,佘旭辉,肖雪霞,黄晓文. 响应面法优化-微波辅助萃取-高效液相色谱法测定农吉利中牡荆素和异牡荆素[J]. 理化检验-化学分册, 2013, 49(2): 129~133
被引情况:
【1】樊轻亚,游国叶, "聚焦微波辅助提取-酸性染料分光光度法测定农吉利中总生物碱",理化检验-化学分册 51, 289-292(2015)
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参考文献
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【12】范华均,肖小华,刘玉竹,等.微波辐射溶剂回流法提取石蒜中石蒜碱、力可拉敏和加兰他敏[J].中山大学学报:自然科学版, 2006,45(3):46-49.
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【14】BEZERRAA M A, SANTELLI R E, OLIVEIRAA E P, et al. Response surface methodology (RSM)as a tool for optimization in analytical chemistry[J]. Talanta, 2008,76(5):965-977.
【2】MUN′IM A, NEGISHI O, OZAWA T, et al. Antioxidative compounds from crotalaria sessiflora[J]. Biosci Biotechnol Biochem, 2003,67(2):410-414.
【3】PRABHAKAR M C, BANO H, KUMAR I, et al. Pharmacological investigations on vitexin[J]. Planta Medica, 1981,43(4):396-403.
【4】KIM J H, LEE B C, SIM G S, et al. The isolation and antioxidative effects of vitexin from Acer palmatum[J]. Arch Pharm Res, 2005,28(2):195-202.
【5】樊轻亚,范华均,黄晓文,等.微波辐射/HPLC测定农吉利中牡荆素和异牡荆素的含量[J].中成药, 2010,32(2):326-329.
【6】肖琳,李静,孙文基.毛细管电泳法测定青叶胆中獐牙菜苦苷和异牡荆素的含量[J].药物分析杂志, 2009,29(12):2040-2043.
【7】冯广卫,李翠兵,廖尚高,等.荭草素和异荭草素、牡荆素和异牡荆素2对碳苷化合物的快速检测与鉴定[J].药物分析杂志, 2011,31(7):1263-1266.
【8】李攻科,杜甫佑,肖小华.微波辅助萃取技术在中药现代化中的应用[J].精细化工, 2007,24(12):1184-1191.
【9】孔娜,邹小兵,黄锐,等.微波辅助萃取/样品前处理联用技术的研究进展[J].分析测试学报, 2010,29(10):1102-1108.
【10】ESKILSSON C S, BJORKLUND E. Analytical-scale microwave-assisted extraction[J]. Journal of Chromatography A, 2000,902:227-250.
【11】KAUFMANNE B, CHRISTEN P. Recent extraction technique for natural products: Microwave-assisted extraction and pressurised solvent extraction[J]. Phytochemical Analysis, 2002,13:105-113.
【12】范华均,肖小华,刘玉竹,等.微波辐射溶剂回流法提取石蒜中石蒜碱、力可拉敏和加兰他敏[J].中山大学学报:自然科学版, 2006,45(3):46-49.
【13】张煜帆,樊轻亚,黄晓文,等.微波辐射溶剂回流提取农吉利中农吉利甲素[J].中国现代应用药学, 2009,26(10):819-823.
【14】BEZERRAA M A, SANTELLI R E, OLIVEIRAA E P, et al. Response surface methodology (RSM)as a tool for optimization in analytical chemistry[J]. Talanta, 2008,76(5):965-977.
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