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目的:建立LC-MS/MS方法,对养血清脑颗粒中15个生物碱成分进行含量测定。方法:采用HSS T3色谱柱(2.1 mm×100 mm,1.8μm),乙腈-0.1%甲酸水为流动相,流速200μL·min~(-1),柱温30℃,电喷雾离子化(ESI),多反应监测离子扫描(MRM),于正离子模式下检测目标化合物,进样量2μL。结果:小檗碱、药根碱、巴马汀、黄连碱、四氢黄连碱、四氢小檗碱、延胡索甲素、延胡索乙素、原阿片碱、钩藤碱、毛钩藤碱、帽柱木菲碱、异帽柱木菲碱、坡绕定、异坡绕定的线性关系良好(r=0.99),各成分加样回收率在89%~107%之间,准确度与精密度良好。结论:该方法操作简便、灵敏度高、分析速度快,可同时测定养血清脑颗粒中多个生物碱成分的含量,有助于快速进行该药品的多成分质量控制。
Objective: To establish a LC-MS / MS method for determination of 15 alkaloids in Yangxue Qingnao Granules. Methods: The mobile phase consisted of HSS T3 column (2.1 mm × 100 mm, 1.8 μm), acetonitrile-0.1% formic acid water, the flow rate was 200 μL · min -1 and the column temperature was 30 ℃. Electrospray ionization (ESI) , Multiple reaction monitoring ion scan (MRM), the target compound was detected in positive ion mode, the injection volume 2μL. Results: Berberine, jatrorrhizine, palmatine, coptisine, tetrahydropiperazine, tetrahydrobiopterin, fomestrin, tetrahydropalmatine, protopine, rhynchophylline, The linear relationship between columnar phenanthrene and isopimamine was better (r = 0.99), and the recoveries of various components were between 89% and 107%. The accuracy and precision good. Conclusion: The method is simple, sensitive, rapid, and can determine the content of alkaloids in Yangxue Qingnao Granules simultaneously, which is helpful for the rapid multi-component quality control of the drug.