UPLC-MS/MS方法同时测定左金丸中23个成分的含量

Simultaneous determination of content of 23 components in Zuojin pills based on UPLC-MS/MS

目的:建立UPLC-MS/MS方法同时测定不同左金丸样品中小檗碱、黄连碱、表小檗碱、药根碱、非洲防己碱、巴马汀、8-氧代-表小檗碱、小檗红碱、木兰花碱、8-氧黄连碱、脱氢紫堇碱、原儿茶酸、5-O-阿魏酰奎尼酸13个黄连成分和吴茱萸碱、吴茱萸次碱、去氢吴茱萸碱、二氢吴茱萸卡品碱、吴茱萸新碱、14-甲酰基二氢吴茱萸次碱、1-甲基-2-十一烷基-4(1H)喹诺酮、1-甲基-2-壬基-4(1H)喹诺酮、茵芋碱、地奥司明10个吴茱萸成分的含量。方法:左金丸80%甲醇水提取液,采用ACQUITY UPLC BEH Shield RP 18(100 mm×2.1 mm, 1.7μm)色谱柱,以乙腈-0.1%甲酸水为流动相,梯度洗脱,流速0.40 mL·min^(-1);质谱采用电喷雾离子源和多反应监测模式采集数据。结果:23个成分在各自的测定范围内线性关系良好(r>0.999 0),平均加样回收率在95.8%~104.0%,精密度、重复性、稳定性均符合要求。结果发现,测定的23个成分在醇提左金丸、水提左金丸和市售左金丸样品中均被检测到,但含量相差较大,如醇提左金丸中小檗碱的含量最高为172.0 mg·g-1,茵芋碱最低为0.021 64 mg·g^(-1)。结论:该方法准确、简便和稳定,可为左金丸相关制剂的质量控制和药效物质基础研究提供参考。

Objective:To establish an UPLC-MS/MS method for the simultaneous determination of 13 components of Coptis chinensis Franch.,including berberine,coptisine,epiberberine,jatrorrihizine,columbamine,palmatine,8-oxo-epiberberine,berberrubine,magnoflorine,8-oxocoptisine,dehydrocorydaline,protocatechuic acid and 5-O-feruloylquinic acid,and 10 components from Euodia rutaecarpa(Juss.)Benth,including evodiamine,rutaecarpine,dehydroevodiamine,dihydroevocarpine,evocarpine,14-formyldihydroxyrutaecarpine,1-methyl-2-undecenyl-4(1H)-quinolone,1-methyl-2-nonyl-4(1H)-quinolone,skimmianine and diosiminin in Zuojin pills.Methods:The 80%methanol extract of Zuojin pills was analyzed on an ACQUITY UPLC BEH Shield RP 18 column(100 mm×2.1 mm,1.7μm),with acetonitrile-water containing 0.1%formic acid as mobile phase at a flow rate of 0.4 mL·min-1.The data was acquired by electrospray ionization source in multiple reaction monitoring mode.Results:23 components showed good linear relationships within their respective ranges(r>0.9990)and the average recoveries were 95.8%-104.0%.And the precision,repeatability and stability all met requirements.These 23 components were all determined in Zuojin pills,and the contents varied greatly.The content of berberine in Zuojin pills extracted by ethanol was the highest of 172.0 mg·g^(-1),while skimmianine was the lowest of 0.02164 mg·g^(-1).Conclusion:The accurate,simple and stable method can be applied for the quality control and pharmacodynamic material basis study of Zuojin pills.