刘雅琳;高慧敏;王智民;张启伟;
LIU Yalin1,2,GAO Huimin,WANG Zhimin,ZHANG Qiwei(1.Institute of Chinese Materia Medica,China Academy of Chinese Medical Sciences,Beijing 100700,China;2.Pharmacy College of Henan University of Traditional Chinese Medicine,Zhengzhou 450008,China)

• 1:中国中医科学院中药研究所
• 2:河南中医学院药学院

摘要(Abstract)：

目的:建立微量马兜铃酸A的标准检测方法,并对目前合法使用的含马兜铃酸A的药材、易与含马兜铃酸药材相混淆的中药材及其中成药进行检测。方法:采用高效液相色谱法,Alltima C18色谱柱(4.6 mm×250 mm,5μm),甲醇-水-乙酸(68∶32∶1.5)为流动相,流速1.0 mL.min-1,检测波长390 nm。结果:马兜铃酸A在0.016~0.51μg线性关系良好,r=0.999 3,最低检测限为4 ng,平均加样回收率为101.2%。采用建立的标准限量检测方法,对11批市售细辛药材和15批中成药样品中马兜铃酸A进行分析;11批细辛中马兜铃酸A的质量分数在3.1~26.6μg.g-1,其中只有3批符合《中国药典》2010年版细辛药材项下的限量规定;15批中成药样品中只有1批检出了马兜铃酸A。结论:方法灵敏度高,重复性好,适合于含痕量马兜铃酸的药材及成药中马兜铃酸A的限量检测。
A HPLC method for limit detection of aristolochic acid A in the Chinese herbs containing aristolochic acid or suspected-containing aristolochic acid and their preparations was established.The samples were analyzed on an Alltima C18 column eluted with methanol-water-acetic acid(68∶32∶1.5) as the mobile phase.Flow rate was at 1.0 mL·min-1 and the detection wavelength was at 390 nm.The calibration curve was linear over the range from 0.016 to 0.51 g(r=0.999 3) and LOD was 4 ng.The average recovery was 101.2% with RSD of 2.01%.The procedures of sample preparation were systematically investigated.The contents of aristolochic acid A in Radix et Rhizoma Asari bought from market or drugstore were fluctuated from 3.1 to 26.6 μg·g-1 and 3 of 11 samples accorded with the quality requirement of current Chinese Pharmacopoeia.Among 15 batches samples of Chinese medicaments,only one sample was found to contain aristolochic acid A.The present investigation shows that the method is sensitive and repeatable and it could be used for the limit detection of aristolochic acid A in the Chinese herbal medicines containing trace amount of aristolochic acid A or suspected-containing aristolochic acid A and their preparations.

关键词(KeyWords)： 马兜铃酸A;限量检测;HPLC
aristolochic acid A;limit detection;HPLC

Abstract:

Keywords:

基金项目(Foundation): 国家中医药管理局中医药科学技术研究专项(06-07ZP54)

作者(Author): 刘雅琳;高慧敏;王智民;张启伟;
LIU Yalin1,2,GAO Huimin,WANG Zhimin,ZHANG Qiwei(1.Institute of Chinese Materia Medica,China Academy of Chinese Medical Sciences,Beijing 100700,China;2.Pharmacy College of Henan University of Traditional Chinese Medicine,Zhengzhou 450008,China)

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