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作 者:郑云枫[1] 阚宏飞 杨阳[1] 严辉[1] 潘苏华[1] 郭海英[1] ZHENG Yun-feng;KAN Hong-fei;YANG Yang;PAN Su-hua;GUO Hai-ying(Nanjing University of Chinese Medicine,Nanjing 210023,China)
出 处:《中国现代中药》2018年第10期1282-1287,共6页Modern Chinese Medicine
基 金:江苏省中医药管理局科技项目(YB2015010);江苏省2017年中药资源普查项目;国家现代农业产业技术体系建设专项资金资助(CARS-21);江苏省高校优势学科建设工程资助项目(PAPD)
摘 要:目的:优化复方银杏叶制剂中银杏酸(GA)的测定方法。方法:以白果新酸对照品结合总银杏酸对照品定位,采用HPLC测定复方银杏叶制剂中5种银杏酸成分总含量,并比较石油醚提取/甲醇溶解、甲醇提取/氯仿萃取和甲醇提取/正己烷萃取法对制剂中银杏酸含量测定结果的影响;进一步以甲醇浓度、溶剂体积、提取时间为影响因素,以总银杏酸含量测定值为评价指标,通过Box-behnken响应面法分析与优化测定方法。结果:甲醇提取/正己烷萃取法对复方银杏叶制剂中总银杏酸的提取精制效果最好。响应面法分析显示,提取溶剂及溶剂体积对总银杏酸含量值具有显著性影响(P <0. 01),最佳提取条件:提取溶剂为85%甲醇,溶剂体积为100 m L,提取时间为1. 8 h,在此条件下方法的平均回收率达97. 7%,精密度RSD为1. 42%。结论:HPLC简便可行,测定结果准确,可用于测定银杏叶提取物及复方制剂中银杏酸的含量测定。Objective: To optimize the content determination method of total ginkgolic acid in compound Ginkgo bi- loba preparation. Methods: Five ginkgolic acids in compound Ginkgo biloba preparation was determined by HPLC using ginkgo acid and total ginkgolic acid as reference standards. The effects of different extraction methods including petroleum ether/methanol extraction, methanol/chloroform extraction and methanol/n-hexane extraction on the determination of total ginkgolic acid were compared. In addition, as the content of total ginkgolic acid was set to be evaluation value, the influence on the technology caused by methanol concentration, extraction volume and extraction time was optimized by using Box- Behnken design and response surface methodology. Results: The results showed that the extracting results were most af- fected by methanol concentration and extraction volume( P 〈 0.01 ). The optimum methanol/n-hexane extraction condi- tions were as follow: the methanol concentration in solvent was 85% , the extraction volume was 100 mL, and the ex- traction time was 1.8 h. The average recovery and relative standard deviation of the method were 97.7% and 1.42% , re- spectively. Conclusion : The method is useful for the quality control of total ginkgolic acid in extract of Ginkgo biloba leav- es and its compound preparations.
关 键 词:复方银杏叶制剂 总银杏酸 含量测定 响应面曲线法 BOX-BEHNKEN设计
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