UPLC-MS/MS检测全粉投料中成药制剂中柴胡掺杂藏柴胡成分方法的研究  

Study on UPLC-MS/MS method for the detection of Radix Bupleuri adulterated Bupleurum marginatum var.stenophyllum in Chinese patent medicine fed with whole powder

作　　者：陈馥[1] 黄俊忠[1] 李华[1] 刘潇潇[1] CHEN Fu;HUANG Jun-zhong;LI Hua;LIU Xiao-xiao(Guangdong Institute for Drug Control,Guangzhou 510700,China)

机构地区：[1]广东省药品检验所,广州510700

出　　处：《药物分析杂志》2023年第7期1245-1254,共10页Chinese Journal of Pharmaceutical Analysis

摘　　要：目的:以藏柴胡特征成分尼泊尔柴胡皂苷k为指标,建立超高效液相色谱-质谱法检测全粉投料中成药制剂中柴胡掺伪藏柴胡成分。方法:采用Agilent Eclipse Plus C18(100 mm×3 mm, 1.8μm)色谱柱,以水(A)-乙腈(B)为流动相,二元梯度洗脱(0~3 min, 75%A→70%A;3~12 min, 70%A→68%A;12~12.5 min, 68%A→10%A;12.5~15.5 min, 10%A),流速0.3 mL·min^(-1),柱温40℃,进样量1μL。采用电喷雾负离子化,多反应监测(MRM)模式,选择m/z 943.5→797.5、943.5→781.5和943.5→635.4为检测离子对。结果:尼泊尔柴胡皂苷k质量浓度在0.05~5μg·mL^(-1)范围与峰面积呈现出良好的线性关系(r=0.996 5),仪器精密度RSD(n=6)为1.4%,掺伪10%藏柴胡参比溶液重复性RSD(n=6)为1.8%,掺伪检测限为1%。对代表性品种逍遥丸、加味逍遥丸、补中益气丸、龙胆泻肝丸进行筛查,结果9批逍遥丸中有2批,8批加味逍遥丸中有4批,10批补中益气丸中有1批,10批龙胆泻肝丸中有2批含尼泊尔柴胡皂苷k超过拟定限度。结论:本方法经过方法学验证,专属性强,灵敏度高,可应用于全粉投料中成药制剂中柴胡掺杂藏柴胡成分的检查。Objective:To establish an UPLC-MS/MS method for the detection of Radix Bupleuri adulterated B.marginatum var.stenophyllum in Chinese patent medicine fed with whole powder,using nepasaikosaponin k,a characteristic component of B.marginatum var.stenophyllum,as an index.Methods:Agilent Eclipse Plus C_(18)column(100 mm×3 mm,1.8μm)was adopted with the mobile phase of water(A)-acetonitrile(B)in gradient mode(0-3 min,75%A→70%A;3-12 min,70%A→68%A;12-12.5 min,68%A→10% A;12.5-15.5 min,10%A),the flow rate was 1.0 mL·min^(-1),the column temperature was 40℃and the injection volume was 1μL.The target compound was analyzed under multiple reaction monitoring(MRM)mode with an ESI~-source operating in negative ion mode,m/z 943.5→797.5,m/z 943.5→781.5,m/z 943.5→635.4 were selected as the detection ion pairs.Results:The linear range of nepasaikosaponin k was 0.05-5μg·mL^(-1)and r was 0.9965,the precision RSD(n=6)of apparatus was 1.4%,the repeatability RSD(n=6)of 10%B.marginatum var.stenophyllum reference solution were 1.8%,the detection limit of adulteration was 1%.The results indicated that 2 out of 9 batches of Xiaoyao pills,4 out of 8 batches of Jiawei Xiaoyao pills,1 out of 10 batches of Buzhong Yiqi pills,2 out of 10 batches of Longdan Xiegan pills contained nepasaikosaponin k exceeding the proposed limit.Conclusion:The method has been verified by methodology,is specific and sensitive,and can be applied to detect the B.marginatum var.stenophyllum which is illegally incorporated in Chinese patent medicine fed with whole powder.

关 键 词：藏柴胡 柴胡 尼泊尔柴胡皂苷k 全粉投料中成药制剂 超高效液相色谱-质谱法 逍遥丸 加味逍遥丸 补中益气丸 龙胆泻肝丸 

分 类 号：R917[医药卫生—药物分析学]