中国临床药理学杂志2017，Vol.33Issue(19)：1949-1953,5.DOI:10.13699/j.cnki.1001-6821.2017.19.028
UPLC-MS/MS法测定积雪草中7种有效成分的含量
Determination of seven active components in Centellaasiatica by UPLC-MS/MS
摘要
Abstract
Objective To develop a rapid and sensitive analytical method for the determination ofseven major compounds (Asiaticoside B,madecassoside,Asiaticoside,madecassic acid,asiatic acid,quercetin,and kaempferol) in Centellaasiaticaby using ultra-performance liquidchromatography coupled with triple-quadrupole tandem mass spectrometry (UPLC-MS/MS) in multiple-reactionmonitoring mode.Methods UPLC-MS/MS assay with positive ion mode was performed on a Waters ACQUITY BEHC18(2.1 mm × 100 mm,1.7 μm) with the mobile phase consisting of acetonitrile and 5 mmol · L-1ammonium acetate in gradient elution at a flow rate of 0.40 mL · min-1 and the column temperature was set at 35 ℃.The positive ion monitoring mode was adopted for MS.The selectivity,linear ranges and limit of quantitation,precision and recovery,repeatability and stability were investigated.Results Underthe optimized chromatographic conditions,good separation for seven target compounds including isomer asiaticoside B and madecassoside were achieved within 8.5 min.Satisfactory linearities were achieved with wide linear ranges,which were 20.00-400.00 ng · mL-1,20.00-400.00 ng · mL-1,20.00-400.00 ng · mL-1,10.00-200.00 ng · mL-1,10.00-200.00 ng· mL-1,50.00-1000.00 ng· mL-1,50.00-1000.00 ng· mL-1 for the determined compounds respectively and fine determination coefficient (r ＞ 0.990 2),the overall recoveries wereranged from 98.3％-100.0％ with the RSD ranging from 1.76％-5.69％.The RSD of precision was between 1.03％-4.67％,for the repeatability and stability,which were between 0.86％-3.21％,0.94％-3.45％,respectively.Conclusion It was the first report about simultaneousanalysis of 7 major components including 5 pentacyclic triterpenes and 2 flavonoids in Centellaasiatica by using UPLC-MS/MS method,which could be used for quality control of Centellaasiatica.关键词
积雪草/UPLC-MS/MS/质量控制Key words
Centellaasiatica/UPLC-MS/MS/quality control分类
医药卫生引用本文复制引用
闫凯,徐艳梅,徐敬朴,段天玮,李德强..UPLC-MS/MS法测定积雪草中7种有效成分的含量[J].中国临床药理学杂志,2017,33(19):1949-1953,5.基金项目
国家自然科学基金资助项目(81603066) （81603066）
河北省自然科学基金资助项目(2015206116) （2015206116）
河北医科大学第二医院科学研究基金资助项目(NO2h2017022) （NO2h2017022）
