LC-MS／MS法研究大承气汤与其君药大黄物质基础间的相关性.pdfVIP

中圊粟科久警学报 136 Journal of China Pharmaceutical University 2008，39(2)：136—141 LC—MS／MS法研究大承气汤与其君药大黄物质基础间的相关性 许风国 ，刘 颖 ，宋 瑞 ，董海娟 ，田 媛 ，张尊建 (中国药科大学 药物质量与安全预警教育部重点实验室；。分析测试中心，南京210009) 摘 要 目的：从物质基础角度研究大承气汤与其君药大黄间的相关性。方法：采用高效液相色谱／串联质谱联用技 术(LC—MS／MS)分析中药经典方剂大承气汤及其君药大黄水提液，研究两者化学成分间的相关性并对主要成分进行结构鉴 定和推测。采用Zorbax SB C 色谱柱，0．2％甲酸一甲醇一乙腈三元梯度洗脱，ESI离子源，负离子模式下采集数据。结果：从 大承气汤中共发现75个成分源于其君药大黄，经与标准品比对可确定其中9个；利用提取离子流技术(EIC)并结合质谱裂 解规律可初步推测其中22个成分的结构。结论：大黄单煎剂中的主要成分在大承气汤中均有所体现；LC—MS／MS技术为中 药方剂物质基础溯源、鉴定，方剂与单味药间的相关性研究提供了一种快速准确的方法。 关键词 大承气汤；大黄：物质基础；高效液相色谱一串联质谱法 中图分类号 R917 文献标识码 A 文章编号 1000—5048(2008)02—0136—06 Correlation of material base between Da--Cheng--Qi decoction and its principal drug rhubarb by LC-MS／MS XU Feng—guo 一，LIU Ying 一，SONG Rui 一，DONG Hai~uan 一，TIAN Yuan 一，ZHANG Zun-jian |Key Laboratory of Drug Quality Control and Pharmacovigilance{China Pharmaceutical University)，Ministry of Education； 。Centerfor Instrumental Analysis，China Pharmaceutical University,Na 210009，China Abstract Aim：To reveal the relationship between Da-·Cheng··Qi decoction and its principal drug rhubarb from the aspect of material base．Methods：After separation on a Zorbax SB Cl R analytical column using 0．2％ formic acid—methanol—acetonitrile gradient elution．negative ESI—MS／MS experiments were performed for Da—Cheng—Qi decoction and rhubarb water extract．respectively．Results：A total of 75 compounds were observed in Da．Cheng． Qi decoction that were originated from its principal drug rhubarb，among which 9 were unambiguously identified by comparing to the standard compounds．and 22 were tentatively identified or deduced according to their MS／MS data in connection with extracted ions chromatographic technique．Conclusion：The present study provides an approach to study the correlation between the traditional Chinese medicine formulae and its medical material from the a