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  

Quality evaluation and content determination of 6 components in Vladimiriasouliei Formula Granules based on UPLC-MS/MS method

作　　者：李芳 严亨波 王育 LI Fang;YAN Hengbo;WANG Yu(The Drug Testing Laboratory of Dazhou Food and Drug Inspection Institute,Dazhou 635000,China;The Traditional Chinese Medicine Laboratory of Dazhou Food and Drug Inspection Institute,Dazhou 635000,China)

机构地区：[1]达州市食品药品检验所药品检测实验室,达州635000 [2]达州市食品药品检验所中药室,达州635000

出　　处：《西北药学杂志》2024年第4期23-28,共6页Northwest Pharmaceutical Journal

摘　　要：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 C_(18)色谱柱(100 mm×2.1 mm,1.8μm)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5μL。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≥0.9970),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。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 C_(18) column(100 mm×2.1 mm,1.8μm)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 5μL.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≥0.9970)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.

关 键 词：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 

分 类 号：R927.2[医药卫生—药学]