质量分析

天王补心丸中炒酸枣仁掺伪情况的研究

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  • 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,南宁 530021
第一作者 Tel:(0771)5827318;E-mail:9994701@qq.com
*罗 轶 Tel:(0771)5828468;E-mail:luoyi20010211@163.com
何颂华 Tel:(0771)5828468;E-mail:hshua3@sina.com

修回日期: 2023-03-08

  网络出版日期: 2024-06-25

Adulteration situation of fried Ziziphi Spinosae Semen in Tianwang Buxin pills

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  • Guangxi Institute for Food and Drug Control, NMPA Key Laboratory for Quality Monitor and Evaluation of Traditional Chinese Medicine, Chinese Material Medica, Nanning 530021, China

Revised date: 2023-03-08

  Online published: 2024-06-25

摘要

目的: 建立天王补心丸中炒酸枣仁的混淆品炒理枣仁的检查方法,测定127批天王补心丸(水蜜丸、大蜜丸)样品,以考察样品中炒酸枣仁的投料状况,予相关生产企业及监管部门警示。方法: 应用高分离度快速液相色谱-三重串联四极杆质谱(UPLC-QQQ/MS)技术,采用Agilent Eclipse C18(100 mm×2.1 mm,1.8 μm)色谱柱,以乙腈-0.1%甲酸水溶液为流动相,梯度洗脱,流速0.2 mL·min-1,柱温30 ℃,进样量1 μL;采用电喷雾离子源(ESI),以多反应监测(MRM)模式进行正离子扫描。结果: 在所设立的色谱条件下,欧鼠李叶碱在相应线性范围内线性关系良好(r>0.999),水蜜丸与大蜜丸中欧鼠李叶碱的加样回收率(n=9)分别为99.13%、97.16%,RSD均<3.3%。用所建立的方法测定127批天王补心丸样品,检出炒理枣仁15批。结论: 天王补心丸中存在以炒理枣仁代替炒酸枣仁投料的情况。

本文引用格式

李丽莉, 吕轶峰, 张慧, 叶倩, 宁崇良, 何颂华, 罗轶 . 天王补心丸中炒酸枣仁掺伪情况的研究[J]. 药物分析杂志, 2023 , 43(4) : 693 -700 . DOI: 10.16155/j.0254-1793.2023.04.19

Abstract

Objective: To establish the detection method of fried Ziziphi Mauritianae Semen in Tianwang Buxin pills to uncover the adulteration situation of fried Ziziphi Spinosae Semen in Tianwang Buxin pills. Methods: The rapid resolution liquid chromatography coupled with triple quadruple mass spectrometry(RRLC-QQQ/MS) was used. The chromatographic separation was achieved on an Agilent Eclipse C18 Column (100 mm×2.1 mm, 1.8 μm), with the mobile phase comprising of 0.1% formic acid solution and acetonitrile at a flow rate of 0.2 mL·min-1 in a gradient elution manner. The column temperature was 30 ℃. The analytes were detected by tandem mass spectrometry with electrospray ionization(ESI) source, and scanned by ESI+ multi-reaction monitoring (MRM)mode. Results: Frangufoline showed good linear relationships within their own ranges (r>0.999). The recoveries of water honey pills and big honey pills were 99.13% and 97.16%(RSD<3.3%,n=9). The method was used to determine 127 batches of Tian Wang Bu Xin Dan samples and fried semen ziziphi spinosae were detected in 15 batches of samples. Conclusion: The mixture of fried Ziziphi Spinosae Semen with Fried Ziziphi Mauritianae Semen exists in Tianwang Buxin pills.

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