LC-MS/MS测定养血清脑颗粒中15个生物碱成分的含量  

Determination of Fifteen Alkaloids in Yangxue Qingnao Granules by LC-MS/MS

作　　者：李文芳[1,2] 王晓明[1] 潘桂湘[1] 尹通[1,2] 郭亚卿[1,2] LI Wenfang WANG Xiaoming PAN Guixiang YIN Tong GUO Yaqing(Tianjin State Key Laboratory of Modern Chinese Medicine,Tianjin University of Traditional Chinese Medicine, Tianjin 300193, China Tianjin International Joint Academy of Biomedicine, Tianjin 300457, China)

机构地区：[1]天津中医药大学天津市现代中药重点实验室省部共建国家重点实验室培育基地,天津300193 [2]天津国际生物医药联合研究院,天津300457

出　　处：《辽宁中医杂志》2017年第10期2144-2146,I0002,共4页Liaoning Journal of Traditional Chinese Medicine

基　　金：国家自然基金项目(81173523;81303182)

摘　　要：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 develop an LC-MS/MS method for the quantitation of fifteen alkaloids in Yangxue Qingnao Granules.Methods：The analysis was performed on a HSS T3 column（2.1 mm×100 mm,1.8 μm） and the flow rate was 200 μL·min^（-1） with acetonitrile -0.1% aqueous formic acid solution as the mobile phase in gradient elution mode.The column temperature was 30 ℃.The detection was performed on a triple quadrupole tandem mass spectrometer with electrospray ionization（ESI）source using multiple reaction monitoring（MRM） mode in the positive mode.Results：Berberine,jatrorrhizine,palmatine,coptisine,tetrahydrocoptisine,tetrahydroberberine,d-corydaline,tetrahydropalmatine,protopine,rhynchophylline,hirsutine,mitraphylline,isomitraphylline,pteropodine,isopteropodine showed good linearity（r=0.99）.The average recoveries ranged from 89% to 107% and better accuracy and precision were achieved.Conclusion：The simple,sensitive and rapid approach has been successfully applied to detect multiple components of Yangxue Qingnao Granules in ways that contributes to the quality control.

关 键 词：养血清脑颗粒 LC-MS/MS 钩藤碱 延胡索乙素 含量测定 

分 类 号：R284[医药卫生—中药学]