十五味黑药丸中5种主要中药成分的定性鉴别及胡椒碱的含量测定.doc

十五味黑药丸中4种活性成分的定性鉴别及胡椒碱的含量测定 胡 婧1，易凡力2，刘松青1 （400038 重庆，第三军医大学西南医院药剂科1；300193天津，天津中医药大学中药学系2） [摘要] 目的 对十五味黑药丸中4种主要中药成分进行定性鉴别并测定胡椒碱的含量。方法 采用薄层色谱法 （ thin layer chromatography, TLC）对方中藏木香、荜茇、黑胡椒、干姜、烈香杜鹃进行定性鉴别；采用高效液相色谱法（HPLC）测定胡椒碱的含量。色谱柱：Phenomenex Luna C18(2)(4.6mm×150mm，5μm)，流动相：甲醇-水（74：26），流速0.8 ml/min，检测波长343nm，柱温35℃。结果 采用TLC均能检出3批十五味黑药丸中的去氢木香内酯、胡椒碱及烈香杜鹃和干姜药材，该鉴别方法专属性强、薄层色谱斑点清晰,阴性对照无干扰；胡椒碱的HPLC色谱峰与其他色谱峰分离良好，进样量在0.021 056～0.105 28 μg范围内呈良好线性关系(r=0.999 8)，平均加样回收率(n=9)为97.76%，3个批次（010624、021008、030323）9个样品中胡椒碱的含量平均值为1.64mg/丸。结论 建立的十五味黑药丸质量标准可用于藏木香、荜茇、黑胡椒、干姜、烈香杜鹃5种中药的成分鉴别及组方中胡椒碱的含量测定。 [关键词] 十五味黑药丸；胡椒碱；薄层色谱法；高效液相色谱法 [中图法分类号] [文献标志码] A Identification of four active ingredients and content determination of Piperine of Shiwuwei Heyaowan pills Hu Jing1，Yi Fanli2，Liu Songqing (1Department of Pharmacy，Southwest Hospital，Third Medical University，Chongqing,400038;2 Tianjin University of Traditional Chinese Medicine,Tianjin, 300070,China) [Abstract] Objective To identification of four active ingredients and content determination of Piperine of Shiwuwei Heyaowan pills. Methods TLC was used for the identification Radix Inulae, Fructus Piperis Longi,Rhizoma zingiberis and Rhododendron Anthopogonoides. HPLC was adopted to identify and determine Piperine in the pills. HPLC conditions: Using Phenomenex Luna C18(2)(4.6mm×150mm,5μm)column was analytic column and Methanol-Water(74:26) was the mobile phase, flow rate at 0.8ml/min,as detector spectrophotometerr set at 343nm,column temperature at 35℃.Results The TLC can detected Dehydrocostuslactone, Piperine , Rhododendron Anthopogonoide and Rhizoma zingiberis in the three baths of Shiwuwei Heyaowan pills. The spot on the TLC plate were clearly. The negative contrast was not disturbed. The method was simple, specific and reproducible. The Chromatographic Peak of Piperine was well isolated. The linear range of Piperine was 0.021 056 – 0.105 28μg(r=0.9998),the average recovery(n=9)was 97.76%, the