LC-MS/MS测定16种市售中药制剂中8种乌头类生物碱的含量  

Determination of 8 Alkaloids in Aconitum species of 16 Chinese traditional patent medicine by LC-MS / MS

作　　者：袁圆[1,2] 王晓明[1] 潘桂湘[1] 张根衍 

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),天津300193 [2]天津国际生物医药联合研究院,天津300457

出　　处：《时珍国医国药》2015年第12期2823-2825,共3页Lishizhen Medicine and Materia Medica Research

基　　金：国家自然基金项目(No.81173523;No.81303182);国家科技支撑计划(No.2011BAI07B08)

摘　　要：目的采用LC-MS/MS方法测定16种含乌头属中药制剂中8种乌头类生物碱含量。方法以90%甲醇-水（水相含0.1%甲酸和2.5 mmol/L醋酸铵水溶液）为流动相,Agilent Zorbax SB-C18色谱柱分离,采用ESI（＋）,MRM监测方法,对16种市售含乌头属中药制剂中苯甲酰乌头原碱、苯甲酰次乌头原碱、苯甲酰新乌头原碱,乌头碱、次乌头碱、新乌头碱,新乌头原碱、乌头原碱进行含量测定。结果上述8种生物碱的线性关系良好,精密度、重复性良好,加样回收率为95.3%～102.3%,不同含乌头属中药制剂中8种生物碱成分的含量差别较大。结论该方法快速、灵敏,可靠,可应用于对乌头属中药制剂的质量控制。Objective The aim of this research was to develop a simple,sensitive LC-MS / MS method for the determination of8 alkaloids in Aconitum species of Chinese traditional patent medicine. Methods After a simple extraction,the separation was performed on an Agilent Zorbax SB-C18 column with a mobile phase consisting of 90% methanol and water（ 0. 1% formic acid and 2. 5 mmol / L ammonium acetate）. A tandem mass spectrometer equipped with electrospray ionization（ ESI） source was used as the detector and was operated in the positive ion mode and multiple reaction monitoring（ MRM）. The method was applied to the determination of benzoylaconine,benzoylhypaconitine,benzoylmesaconitine,aconitine,hypaconitine,mesaconitine,mesaconine and aconitine. Results Good linearity,precision and accuracy were obtained at the concentration ranges under investigation with repeatability was less than 6%. The mean recoveries ranged from 95. 3% to 102. 3%. In addition,we found a big difference in the content of alkaloids in various Chinese traditional patent medicine. Conclusion LC-MS / MS method is sensitive and rapid in the determination of Aconitum of Chinese traditional patent medicine and can be applied to the quality control of aconitum species.

关 键 词：乌头类生物碱 LC-MS/MS 中成药 质量控制 

分 类 号：R284.1[医药卫生—中药学]