TLC联合UPLC-QQQ-MS分析天王补心丸中4种外源性污染成分

doi:10.19803/j.1672-8629.20230572

中国药物警戒 ›› 2024, Vol. 21 ›› Issue (2): 156-162.
DOI: 10.19803/j.1672-8629.20230572

TLC联合UPLC-QQQ-MS分析天王补心丸中4种外源性污染成分

张赞, 张慧, 何颂华^*, 罗轶^#

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

收稿日期:2023-09-14 出版日期:2024-02-15 发布日期:2024-02-06
通讯作者: ^*何颂华,男,本科,副主任药师,中药材及其制剂检测分析。E-mail：hshua3@sina.com。^#为共同通信作者。
作者简介:张赞,男,本科,副主任药师,药品检验和药物质量研究。
基金资助:
广西科技重大专项（桂科AA22096019）

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

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

Received:2023-09-14 Online:2024-02-15 Published:2024-02-06

摘要/Abstract

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、0.88~87.75 ng·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。

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

Abstract: 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 3.2~24.8 μg·g^-1, respectively. Conclusion This method is simple, accurate, and highly specific, which can provide reference for quality control of Tianwang Buxin pills.

Key words: Tianwang Buxin pills, thin layer chromatography, ultra high performance liquid chromatography, triple quadrupole mass spectrometry, exogenously, polluted

中图分类号:

R927.11

张赞, 张慧, 何颂华, 罗轶. TLC联合UPLC-QQQ-MS分析天王补心丸中4种外源性污染成分[J]. 中国药物警戒, 2024, 21(2): 156-162.

ZHANG Zan, ZHANG Hui, HE Songhua, LUO Yi. Four exogenously-polluted components in Tianwang Buxin pills analyzed via TLC and UPLC-QQQ-MS[J]. Chinese Journal of Pharmacovigilance, 2024, 21(2): 156-162.

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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

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