首页|基于UPLC-MS/MS测定川木香配方颗粒中6种成分的含量及质量评价

基于UPLC-MS/MS测定川木香配方颗粒中6种成分的含量及质量评价

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目的 建立超高效液相色谱串联质谱(ultra performance liquid chromatograpy-tandem mass spectrometry,UPLC-MS/MS)同时测定川木香配方颗粒中紫丁香苷、新绿原酸、绿原酸、隐绿原酸、木香烃内酯和去氢木香烃内酯含量的方法,并对川木香配方颗粒的质量进行综合评价。方法 用Agilent SB C18色谱柱(100 mm×2。1 mm,1。8 μm)进行分离;以乙腈-3 mL·L-1甲酸为流动相,梯度洗脱;柱温为35℃;流速为0。3 mL·min-1;进样量为5 μL。质谱用电喷雾(electrospray ionization,ESI)离子源,多反应监测模式(multiple-reaction monitoring,MRM)正、负离子同时扫描,对川木香配方颗粒进行定量分析。结果 川木香配方颗粒6种成分在各自的质量浓度范围内线性关系良好(r≥0。997 0),精密度RSD值<2。56%,重复性RSD值<2。15%,稳定性RSD值<3。62%,平均回收率在96。23%~103。41%之间。结论 该方法灵敏、准确、重复性好,可为川木香配方颗粒中6种成分的含量测定及川木香质量标准的完善和提高提供参考。
Quality evaluation and content determination of 6 components in Vladimiriasouliei Formula Granules based on UPLC-MS/MS method
Objective To establish a method for the simultaneous determination of syringin,neochlorogenic acid,chlorogenic acid,cryptochlorogenic,costunolide and dehydrocostus lactone in Vladimiriasouliei Formula Granules by ultra performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS),and to evaluate their quality comprehensively.Methods An Agilent SB C18 column(100 mm×2.1 mm,1.8 μm)was used to separate the samples with gradient elution of acetonitrile-3 mL·L-1 formic acid as mobile phase,flow rate of 0.3 mL·min-1,column temperature of 35℃and the injection volume of 5 μL.The 6 compounds were quantitatively analyzed with electrospray ionization(ESI)ion source and multiple-reaction monitoring(MRM)scanning in positive and negative ions mode,simultaneously.Results The 6 components of Vladimiriasouliei Formula Granules showed good linear relationship(r≥0.997 0)with their peak areas in their respective concentration ranges,with respective RSDs of precision less than 2.56%,RSDs of repeatability less than 2.15%and the RSDs of stability less than 3.62%.The average recoveries were between 96.23%and 103.41%.Conclusion The method is sensitive,accurate,and reproducible which can be used for the determination of the 6 components in Vladimiriasouliei Formula Granules and the improvement of the quality standard of Vladimiriasouliei.

Vladimiriasoulieiformula granulescontent determinationquality controlUPLC-MS/MS

李芳、严亨波、王育

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达州市食品药品检验所药品检测实验室,达州 635000

达州市食品药品检验所中药室,达州 635000

川木香 配方颗粒 含量测定 质量评价 超高效液相色谱串联质谱法

2024

西北药学杂志
西安交通大学,陕西省药学会

西北药学杂志

CSTPCD
影响因子:0.912
ISSN:1004-2407
年,卷(期):2024.39(4)