单面针HPLC指纹图谱及质量标准研究  

Study on HPLC Fingerprint and Quality Standard of Zanthoxylum Dissitum

作　　者：刘倩倩 雷思敏[1,2] 胡玉珍 夏伯候[1,2] 林艳 林丽美[1,2] 龚云 张鹏[3] 吴萍 LIU Qianqian;LEI Simin;HU Yuzhen;XIA Bohou;LIN Yan;LIN Limei;GONG Yun;ZHANG Peng;WU Ping(College of Pharmacy,Hunan University of Chinese Medicine,Changsha 410208,China;Key Laboratory for Quality Evaluation of Bulk Herbs of Hunan Province,Changsha 410208,China;Zhuzhou Qianjin Pharmaceutical Co.,Ltd,Zhuzhou 412003,China)

机构地区：[1]湖南中医药大学药学院,湖南长沙410208 [2]湘产大宗药材品质评价湖南省重点实验室,湖南长沙410208 [3]株洲千金药业股份有限公司,湖南株洲412003

出　　处：《中国中医药信息杂志》2020年第10期73-79,共7页Chinese Journal of Information on Traditional Chinese Medicine

基　　金：国家中药标准化项目(ZYBZH-C-HUN-21);湖南省科技计划(2015SK1001);长沙市科技计划(kq1706056、kq1804027);湖南中医药大学“十三五”一级学科(2018年)。

摘　　要：目的建立单面针药材的特征指纹图谱,测定单面针中木兰花碱、水分、总灰分、酸不溶性灰分、浸出物含量,以控制单面针药材质量,并为与两面针的区别提供参考。方法采用HPLC建立基于区分两面针的单面针指纹图谱,色谱柱为Athena C18,120A(4.6 mm×250 mm,5μm),以甲醇-0.1%甲酸水溶液为流动相,梯度洗脱,流速1 mL/min,进样量10μL,柱温30℃,检测波长283 nm。采用主成分分析及正交偏最小二乘-判别分析对单面针和两面针指纹图谱进行比较,筛选其差异标志物,并利用对照品进行标志物鉴定和含量测定。参照2015年版《中华人民共和国药典》(四部)通则方法测定单面针的水分、总灰分、酸不溶性灰分、浸出物含量。结果建立了单面针特征指纹图谱,发现了区分单面针与两面针的11个标志性化合物,指认出其中1个标志物为木兰花碱。木兰花碱在0.48~5.76μg范围内呈良好线性关系(r=1),平均加样回收率为97.23%,RSD=1.31%,样品含量为2.2273~21.0272 mg/g。单面针中水分、总灰分、酸不溶性灰分、水溶性浸出物、醇溶性浸出物含量分别为5.016%~10.910%、2.487%~5.973%、0.027%~0.147%、0.548%~2.512%、0.332%~2.113%。结论本研究建立的方法操作简便,准确性及重复性好,可用于评价单面针药材的质量。Objective To establish a quality-control method of Zanthoxylum dissitum,including establishment of characteristic fingerprint and determination of the contents of magnoflorine,moisture,total ash,acid insoluble ash and extract;To provide reference for distinguishing Zanthoxylum dissitum from Zanthoxylum nitidum.Methods Fingerprints of Zanthoxylum dissitum based on HPLC method was established on a Waters Athena C18,120 A column(4.6 mm×250 mm,5μm)at 30℃,with a gradient mobile phase composed of methanol and 0.1%formic acid at a flow rate of 0.3 mL/min.The detection wavelength was 283 nm.Principal component analysis and orthogonal partial least squares discriminate analysis were adopted to screen differential markers between Zanthoxylum dissitum and Zanthoxylum nitidum.The identification and determination of markers were carried out by comparing with real standard products.The contents of water,total ash,acid insoluble ash and extract were determined according to the general rule in four part of Chinese Pharmacopoeia(2015 edition).Results Characteristic fingerprints of Zanthoxylum dissitum were established.11 mark compounds were found to distinguish Zanthoxylum dissitum and Zanthoxylum nitidum.Among which,magnoflorine was identified.The magnoflorine showed a good linear response in the range of 0.48-5.76μg(r=1).The average of recovery was 97.23%with RSD=1.31%.The contents of magnoflorine in the samples of Zanthoxylum dissitum were 2.2273-21.0272 mg/g,and the result of water,total ash,acid insoluble ash,water soluble extract and ethanol soluble extract of Zanthoxylum dissitum were 5.016%-10.910%,2.487%-5.973%,0.027%-0.147%,0.548%-2.512%and 0.332%-2.113%,respectively.Conclusion The established method is simple,accurate and reproducible,and can be used to evaluate the quality of Zanthoxylum dissitum.

关 键 词：单面针 高效液相色谱法 质量标准 木兰花碱 

分 类 号：R284.1[医药卫生—中药学]