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HPLC测定钩藤中钩藤碱和异钩藤碱的方法学探讨
引用本文:杨秀娟,洪燕龙,吴飞,阮克锋,冯怡.HPLC测定钩藤中钩藤碱和异钩藤碱的方法学探讨[J].中国中药杂志,2013,38(5):720-724.
作者姓名:杨秀娟  洪燕龙  吴飞  阮克锋  冯怡
作者单位:1. 上海中医药大学中药现代制剂技术教育部工程研究中心,上海201203;上海张江中药现代制剂技术工程研究中心,上海201203
2. 上海张江中药现代制剂技术工程研究中心,上海,201203
基金项目:上海市科委中药现代化专项(10DZ1973000);上海市自然科学基金项目(09ZR1429600);上海市教委创新项目(10YZ57);上海市教委重点学科项目(J50302)
摘    要:目的:探讨钩藤中钩藤碱和异钩藤碱的HPLC含量测定方法.方法:采用RP-HPLC,对钩藤中钩藤碱和异钩藤碱的HPLC含量测定方法学进行考察,同时采用HPLC-ESI-MS研究钩藤碱和异钩藤碱在加热过程中的化学成分转化情况.结果:钩藤碱在0.064~5.100 mg线性关系良好,精密度良好;当样品采用同流提取时,平均加样回收率87.51%~88.83%,提取回收率12.60%;当样品采用超声提取时,平均加样回收率99.48% ~ 103.2%,提取回收率47.08%.异钩藤碱在0.064~5.110 mg线性关系良好,精密度良好;当样品采用回流提取时,平均加样回收率107.9%~113.9%,提取回收率40.00%,当样品采用超声提取时,平均加样回收率97.00%~99.59%,提取回收率51.03%.质谱分析结果表明回收率不合格的原因是钩藤碱在提取过程中大部分转化为异钩藤碱,有一小部分转化为未知成分;异钩藤碱在提取过程中转化为钩藤碱、去氢钩藤碱、异去氢钩藤碱及22-O-β-D-glucopyranosyl isocorynoxeinic acid4种成分.结论:HPLC测定钩藤中钩藤碱和异钩藤碱宜采用超声提取法,并应注意同收率问题.

关 键 词:钩藤  钩藤碱  异钩藤碱  HPLC
收稿时间:2012/9/22 0:00:00

Determination of rhynchophylline and isorhynchophylline in Uncaria rhynchophylla by HPLC
YANG Xiu-juan,HONG Yan-long,WU Fei,RUAN Ke-feng and FENG Yi.Determination of rhynchophylline and isorhynchophylline in Uncaria rhynchophylla by HPLC[J].China Journal of Chinese Materia Medica,2013,38(5):720-724.
Authors:YANG Xiu-juan  HONG Yan-long  WU Fei  RUAN Ke-feng and FENG Yi
Institution:Engineering Research Center of Modern Preparation Technology of Traditional Chinese Medicine, Ministry of Education, Shanghai University of Traditional Chinese Medicine, Shanghai 201203, China;Engineering Research Center of Modern Preparation Technology of Traditional Chinese Medicine of Zhangjiang, Shanghai 201203, China;Engineering Research Center of Modern Preparation Technology of Traditional Chinese Medicine of Zhangjiang, Shanghai 201203, China;Engineering Research Center of Modern Preparation Technology of Traditional Chinese Medicine, Ministry of Education, Shanghai University of Traditional Chinese Medicine, Shanghai 201203, China;Engineering Research Center of Modern Preparation Technology of Traditional Chinese Medicine of Zhangjiang, Shanghai 201203, China;Engineering Research Center of Modern Preparation Technology of Traditional Chinese Medicine, Ministry of Education, Shanghai University of Traditional Chinese Medicine, Shanghai 201203, China;Engineering Research Center of Modern Preparation Technology of Traditional Chinese Medicine of Zhangjiang, Shanghai 201203, China;Engineering Research Center of Modern Preparation Technology of Traditional Chinese Medicine, Ministry of Education, Shanghai University of Traditional Chinese Medicine, Shanghai 201203, China;Engineering Research Center of Modern Preparation Technology of Traditional Chinese Medicine of Zhangjiang, Shanghai 201203, China
Abstract:
Keywords:Uncaria rhynchophylla  rhynchophylline  isorhynchophylline  HPLC
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