UPLC-MS/MS方法同时测定百咳宁颗粒中6种主要有效成分  

Simultaneous determination of six components in Baikening Granules by UPLC-MS/MS

作　　者：李瑞宏[1] 房桂珍[2] 安娜[1] 冯超[1] 祁金龙[3] 张海林[3] 

机构地区：[1]河北省儿童医院,河北石家庄050013 [2]河北医科大学生物医学工程中心,河北石家庄050017 [3]河北医科大学药理学教研室,河北石家庄050017

出　　处：《中草药》2016年第1期76-80,共5页Chinese Traditional and Herbal Drugs

基　　金：国家自然科学基金资助项目(21402139);河北省自然科学基金资助项目(H2013206048);河北省教育厅优秀青年基金资助项目(YQ2013033);河北省医学科学研究重点课题计划项目(20150560);河北省食品药品监督管理局(重点)科技项目(ZD2015023)

摘　　要：目的建立UPLC-MS/MS方法同时测定百咳宁颗粒中6种主要有效成分（靛玉红、贝母素甲、贝母素乙、银杏内酯A、银杏内酯B和银杏内酯C）。方法百咳宁颗粒经氯仿-甲醇溶剂索氏提取后进样,采用正负离子切换的多反应监测（MRM）模式同时测定百咳宁颗粒中的靛玉红,2种贝母素和3种银杏内酯类成分。色谱柱为Inertsutain C_（18）（75 mm×3.0 mm,2μm）柱,流动相为甲醇-乙腈-2 mmol/L乙酸铵水溶液,梯度洗脱,分析时间为6 min。结果所测6种主要有效成分在测定浓度范围内线性关系良好,r均大于0.995 8;精密度、重复性和稳定性良好;平均加样回收率为96.5%~105.1%,RSD≤4.2%。结论本法简单快捷、灵敏度高、专属性好,可用于百咳宁颗粒中6中主要有效成分的定量控制,除靛玉红外,其他5种成分均为处方中首次测定,百咳宁颗粒中银杏内酯类成分的量较低。Objective To develop an ultra-high performance liquid chromatography-tandem mass spectrometry（UPLC-MS/MS） method for simultaneous determination of six components（indirubin, peimine, peiminine, ginkalide A, ginkalide B, and ginkalide C） in Baikening Granules. Methods Preparing the samples solution by Soxhlet＇s extraction using methanol-chloroform as solvent, and multiple reaction monitoring（MRM） with a polarity-switching electrospray ionization（ESI） source between positive and negative modes was used for the quantification of indirubin, two peimisines, and three bilobalides. The detection was performed on an Inertsutain C_（18） column（75 mm × 3.0 mm, 2 μm） using a mobile phase consisted of methanol-acetonitrile and 2 mmol/L ammonium acetate water solution with gradient elution lasting 6 min. Results All of the analytes showed good linearity（r ≥ 0.995 8） in the tested ranges. The precision, repeatability, and stability of the method were good for the six components. The average recoveries were in the range of 96.5%—105.1% with relative standard deviations（RSD） ≤ 4.2%. Conclusion The new established polarity-switching LC-MS-MS method has been proven to be highly sensitive and effective in evaluating the quality of Baikening Granules, and peimine, peiminine, ginkalide A, ginkalide B, and ginkalide C are quantified in this drug for the first time.

关 键 词：UPLC-MS/MS 百咳宁颗粒 靛玉红 贝母素甲 贝母素乙 银杏内酯A 银杏内酯B 银杏内酯C 

分 类 号：R286.02[医药卫生—中药学]