UPLC-MS/MS法同时测定注射用益气复脉(冻干)中13种成分  

Simultaneous analysis on 13 components in Yiqi Fumai Injection(freeze-dried) by UPLC-MS/MS method

作　　者：乔晓莉[1] 肖学凤[2] 周大铮[3] 叶正良[3] 付淑军[4] 阎姝[1] 刘昌孝[2,5] 

机构地区：[1]天津市南开医院,天津300100 [2]天津中医药大学,天津300193 [3]天津天士力之骄药业有限公司,天津300410 [4]天津国际生物医药联合研究院,天津300457 [5]天津药物研究院,天津300193

出　　处：《中草药》2014年第23期3402-3407,共6页Chinese Traditional and Herbal Drugs

基　　金：重大新药创制专项(2013ZX09402202)

摘　　要：目的建立同时测定注射用益气复脉（冻干）（YFI）中人参皂苷类（人参皂苷Rb1、Re、Rg1、Rc、Rd、Rf、Rg3、F2和三七皂苷R1）和木脂素类（五味子醇甲、五味子醇乙、五味子甲素和五味子乙素）共13种成分的UPLC-MS/MS分析方法,并对YFI中上述成分进行定量分析。方法采用液质联用法,应用C18柱,流动相为含0.1%甲酸的水溶液和含0.1%甲酸的甲醇溶液梯度洗脱,质谱采用正离子模式,多反应监测扫描。结果 YFI中13种成分线性关系、精密度、稳定性、重复性均符合方法学测定要求,加样回收率为98.28%~101.08%。应用所建立的方法测定了5批次YFI中人参皂苷类和木脂素类共13个成分的量。结论所建立的用于同时测定YFI中13种成分的分析方法简单、重复性好、准确可靠,可为YFI质量控制提供依据。Objective To establish a UPLC-MS/MS analytical method for the simultaneous analysis of ginsenosides（ginsenosides Rb1, Re, Rg1, Rc, Rd, Rf, Rg3, F2, and notoginsenoside R1） and lignans（gomisin A, schisandrol B, deoxyschizandrin, and schisandrin B） in Yiqi Fumai Injection（freeze-dried）（YFI）, and measure the contents of these constituents in YFI. Methods Quantitative research of 13 components in YFI was done by reversed-phase liquid chromatography on a C18 column using a gradient elution（0.1% formic acid in water and 0.1% formic acid in methanol）. A triple quadrupole mass spectrometer operating in positive electrospray ionization mode with multiple reaction monitoring was used. Results Thirteen components in YFI have good linear relationship, precision, stability, and repeatability according to the requirements of the methodology determination. The recoveries were 98.28%—101.08%. The 13 components in three batches of YFI were determined by UPLC-MS/MS method. Conclusion The developed UPLC-MS/MS method is simple, sensitive, and accurate, and has good repeatability. The 13 components in YFI could be rapidly and accurately quantified by UPLC-MS/MS, which provides the helpful information for the comprehensive quality evaluation of YFI.

关 键 词：UPLC-MS/MS 注射用益气复脉(冻干) 人参皂苷类化合物 木脂素类化合物 三七皂苷R1 五味子醇甲 五味子醇乙 五味子甲素 五味子乙素 

分 类 号：R286.02[医药卫生—中药学]