TLC联合UPLC-QQQ-MS分析天王补心丸中4种外源性污染成分  

Four exogenously-polluted components in Tianwang Buxin pills analyzed via TLC and UPLC-QQQ-MS

作　　者：张赞 张慧 何颂华 罗轶 ZHANG Zan;ZHANG Hui;HE Songhua;LUO Yi(Guangxi Institute for Food and Drug Control,NMPA Key Laboratory for Quality Monitoring and Evaluation of Traditional Chinese Medicine,Chinese Materia Medica,Nanning Guangxi 530021,China)

机构地区：[1]广西壮族自治区食品药品检验所,国家药品监督管理局中药材质量监测与评价重点实验室,广西南宁530021

出　　处：《中国药物警戒》2024年第2期156-162,共7页Chinese Journal of Pharmacovigilance

基　　金：广西科技重大专项(桂科AA22096019)。

摘　　要：目的对天王补心丸质量分析中发现的异常成分进行研究,建立薄层色谱(TLC)、超高效液相色谱—三重四极杆质谱(UPLC-QQQ-MS)同时测定天王补心丸中盐酸小檗碱、表小檗碱、盐酸黄连碱、盐酸巴马汀等4种外源性污染成分的分析方法。方法采用TLC法,通过优化展开系统,对158批样品进行定性鉴别;针对异常斑点,采用HPLC-Q/TOF-MS进行成分鉴定确认;采用UPLC-QQQ-MS进行定量分析。结果158批天王补心丸样品中有9批检出盐酸小檗碱、表小檗碱、盐酸黄连碱、盐酸巴马汀等4种外源性污染成分,分别在0.97~483.34、0.98~98.49、1.00~100.50、0.88~87.75ng·mL^(-1)内呈线性,回收率为99.30%~103.99%,平均标准偏差(RSD)为0.90%~2.62%(n=6),9批样品中上述4种成分的含量分别为20.3~104.1、1.0~17.6、0.4~30.6、3.2~24.8μg·g^(-1)。结论该方法简便、准确、专属性强,可为天王补心丸的质量控制提供参考。Objective To tentatively study abnormal components of Tianwang Buxin pills on sale that were found in quality analysis and establish an analytical method for simultaneous determination of four exogenously-polluted components using TLC and UPLC-QQQ-MS.Methods One hundred and fifty-eight batches of samples of Tianwang Buxin pills were qualitatively identified by using the TLC method and optimizing the unfolding system.For abnormal spots,HPLC-Q/TOF-MS was used for identification and confirmation of components.UPLC-QQQ-MS was adopted for quantitative analysis.Results Among the 158 batches of samples,four types of exogenously-polluted components,including Berberine hydrochloride,Epiberberine,Coptisine hydrochloride and Palmatine chloride,were detected in nine batches.These four types of components were linear within the range of 0.97~483.34,0.98~98.49,1.00~100.50 and 0.88~87.75 ng·mL^(-1),respectively.The recovery ranged from 99.30%to 103.99%,and the RSD from 0.90%to 2.62%(n=6).The contents of these components were 20.3~104.1,1.0~17.6,0.4~30.6 and 3.2~24.8μg·g-1,respectively.Conclusion This method is simple,accurate,and highly specific,which can provide reference for quality control of Tianwang Buxin pills.

关 键 词：天王补心丸 薄层色谱 超高效液相色谱 三重四极杆质谱 外源性 污染 

分 类 号：R927.11[医药卫生—药学]