[关键词]
[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 C18(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0.9958;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。
[Key word]
[Abstract]
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 C18 column(75 mm×3.0 mm, 2μm) 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 ≥ 0.9958) 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.
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[基金项目]
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)