基于UPLC-MS/MS技术检查银柴颗粒中柴胡掺伪的鉴别研究

陈馥; 黄俊忠; 徐万帮; 刘潇潇

文章摘要

陈馥,黄俊忠,徐万帮,刘潇潇.基于UPLC-MS/MS技术检查银柴颗粒中柴胡掺伪的鉴别研究[J].中国药事,2023,(4):426-433

基于UPLC-MS/MS技术检查银柴颗粒中柴胡掺伪的鉴别研究

Identifi cation of Bupleurum chinense in Yinchai Granules by UPLC-MS/MS

DOI：10.16153/j.1002-7777.2023.04.009

中文关键词: 尼泊尔柴胡皂苷K 藏柴胡银柴颗粒高效液相色谱-质谱法

英文关键词: Nepasaikosaponin K Bupleurum marginatum var. stenophyllum Yinchai granules UPLC-MS/MS

基金项目:

作者	单位
陈馥	广东省药品检验所,国家药品监督管理局药品快速检验技术重点实验室,广东省药品监督管理局粤港澳大湾区中药标准研究重点实验室,广州 510700
黄俊忠	广东省药品检验所,国家药品监督管理局药品快速检验技术重点实验室,广东省药品监督管理局粤港澳大湾区中药标准研究重点实验室,广州 510700
徐万帮	广东省药品检验所,国家药品监督管理局药品快速检验技术重点实验室,广东省药品监督管理局粤港澳大湾区中药标准研究重点实验室,广州 510700
刘潇潇	广东省药品检验所,国家药品监督管理局药品快速检验技术重点实验室,广东省药品监督管理局粤港澳大湾区中药标准研究重点实验室,广州 510700

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中文摘要:

目的：建立银柴颗粒中藏柴胡的检查方法，考察生产企业是否存在使用藏柴胡代替柴胡投料的现象。方法：采用高效液相色谱-质谱法，选择Agilent Eclipse Plus C₁₈(100 mm×3 mm，1.8μm)色谱柱；流动相为乙腈(A)-水(B)，二元梯度洗脱，流速0.3 mL·min^-1，柱温 40 ℃；采用质谱检测器，电喷雾负离子模式(ESI- )，进行多反应监测(MRM)，选择m/z 943.5→797.5、m/z 943.5→635.4和m/z 943.5→781.5为检测离子对。结果：尼泊尔柴胡皂苷K在0.1~5μg·mL-1浓度范围与峰面积呈现出良好的线性关系(r=0.9920)，仪器精密度RSD(n=6)为0.57%，样品重复性RSD(n=6)为0.95%。以掺杂藏柴胡不得过10%为限度，对27批银柴颗粒样品进行筛查，结果4批银柴颗粒分别掺杂藏柴胡59%、21%、 32%、71%，超过拟定限度。结论：该方法经过方法学验证，灵敏、准确，可作为银柴颗粒中柴胡掺杂藏柴胡的检查方法，为打击藏柴胡掺伪提供有力技术支持。

英文摘要:

Objective：To establish the identification method of Bupleurum marginatum var. stenophyllum in Yinchai granules and investigate whether there exists a phenomenon of using B. marginatum var. stenophyllum to replace B. chinense in the manufacture enterprises. Methods：UPLC-MS/MS was used with Agilent Eclipse Plus C₁₈(100 mm ×3 mm, 1.8 μm) as analytical column, acetonitrile (A)-water(B) as a phase of step gradient elution, the fl ow rate was 0.3 mL·min^-1, the column themperature was 40 ℃. 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→635.4, m/z 943.5→781.5 were selected as the detection ion pairs. Results：Nepasaikosaponin K showed a good linear relationship in the range of 0.1-5 μg·mL–1 with a r at 0.9920, the precision RSD (n=6) of apparatus was 0.57%, the repeatability RSD (n=6) of sample was 0.95%. Total of 27 batches of Yinchai granule samples were screened with the limit that the doping of B. marginatum var. stenophyllum should not exceed 10%. The results showed that the doping of B. marginatum var. stenophyllum in 4 batches of Yinchai granules was 59%, 21%, 32% and 71%, which exceeded the proposed limit. Conclusion:：The method has been verified by methodology, it is sensitive and accurate, and could be applied to detect the B. marginatum var. stenophyllum in the Yinchai granules.

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