柴胡属饮片中藏柴胡掺伪检测方法研究  

Analytical method of Bupleurum marginatum var.stenophyllum adulteration in Bupleurum

作　　者：赵丹彤 高一军 毕天琛 王素香 郑兆显 林永强 ZHAO Dantong;GAO Yijun;BI Tianchen;WANG Suxiang;ZHENG Zhaoxian;LIN Yongqiang(Heze Institute for Food and Drug Control,Heze 274000,China;Heze Municipal Hospital,Heze 274031,China;Shandong Institute for Food and Drug Control,Shandong Engineering Laboratory for Standard Innovation and Quality Evaluation of TCM,Jinan 250101,China)

机构地区：[1]菏泽市食品药品检验检测研究院,山东菏泽274000 [2]菏泽市立医院,山东菏泽274031 [3]山东省食品药品检验研究院/山东省中药标准创新与质量评价工程实验室,山东济南250101

出　　处：《药学研究》2022年第10期653-658,663,共7页Journal of Pharmaceutical Research

基　　金：山东省重点研发计划(No.2021CXGC010511);山东省人文社会科学课题(No.2021-YYGL-44)。

摘　　要：目的以Nepasaikosaponin K为指标,建立柴胡属饮片中藏柴胡掺伪检测方法。方法采用高效液相色谱-串联质谱技术(HPLC-MS/MS),电喷雾负离子多反应监测模式,以m/z 943.6→635.5、m/z 943.6→797.4、m/z 943.6→781.5为特征离子对,对北柴胡、南柴胡、锥叶柴胡、竹叶柴胡和藏柴胡等5种常见柴胡属饮片中Nepasaikosaponin K含量进行检测。进一步考察Nepasaikosaponin K定量离子对峰面积与藏柴胡掺伪比例之间线性关系,建立柴胡属饮片中藏柴胡掺伪比例计算公式,并以Nepasaikosaponin K为指标,开展藏柴胡掺伪限度研究。结果Nepasaikosaponin K在藏柴胡中含量约为其他种柴胡的25~140倍。藏柴胡掺伪比例为0~100%范围内的混合样品中,定量离子对m/z 943.6→635.5峰面积与掺伪比例之间的线性关系良好。不同柴胡属掺伪模拟样品的计算掺伪量与实际掺伪量偏差在0.6%~1.4%之间。3批市售疑似掺伪北柴胡饮片中藏柴胡掺伪比例分别为14%、16%和27%。结论该分析方法专属性强,灵敏度高,测定结果准确,为柴胡饮片中藏柴胡的掺伪情况筛查与评价提供依据,同时为其他中药饮片的掺伪情况分析提供新的思路与方法。Objective To developed an analytical method of Bupleurum marginatum var.stenophyllum adulteration in Bupleurum with Nepasaikosaponin K as an index.Methods The HPLC-MS/MS method was used to detect the content of Nepasaikosaponin K in five kinds of Bupleurum medicinal materials such as Bupleurum chinense,Bupleurum scorzonerifolium,Bupleurum bicaule,Bupleurum marginatum and Bupleurum marginatum var.stenophyllum,using electrospray negative ion multi reaction monitoring mode with m/z 943.6→635.5,m/z 943.6→797.4,m/z 943.6→781.5 as the characteristic ion pair.Further investigated the linear relationship between the peak area of Nepasaikosaponin K quantitative ion pair and the adulteration proportion of Bupleurum marginatum var.stenophyllum,established the adulteration proportion calculation formula of Bupleurum marginatum var.stenophyllum in Bupleurum,and take Nepasaikosaponin K as the index to study the adulteration limit.Results The content of Nepasaikosaponin K in Bupleurum marginatum var.stenophyllum was about 25~140 times that of other Bupleurum species.There was a good linear relationship between the quantitative ion pairs of m/z 943.6→635.5 peak area and the adulteration ratio of Bupleurum marginatum var.stenophyllum mixed samples with adulteration proportion ranging from 0 to 100%.The deviation between the calculated adulteration amount and the actual adulteration amount of different Bupleurum adulteration simulation samples was between 0.6%~1.4%.The adulteration rates of Bupleurum marginatum var.stenophyllum in three batches of commercial suspected adulterated Bupleurum chinense were 14%,16%and 27%respectively.Conclusion The analytical method had strong specificity,high sensitivity and accurate determination results,which can provide a basis for screening and evaluation of Bupleurum marginatum var.stenophyllum adulteration in Bupleurum,and also provide a new idea and method for analysis of adulteration of other traditional Chinese medicines.

关 键 词：柴胡 藏柴胡 Nepasaikosaponin K 掺伪 高效液相色谱-串联质谱技术 

分 类 号：R284.1[医药卫生—中药学]