UHPLC-ESI-MS/MS同时测定心安宁胶囊中的5种药效成分

Simultaneous Determination of 5 Components in Xin'anning Capsules by UHPLC-ESI-MS/MS

关键词:  液质联用  心安宁胶囊  葛根素  二苯乙烯苷  金丝桃苷  槲皮素  齐墩果酸  多重反应监测

Key words:  UHPLC-ESI-MS/MS  Xin'anning capsules  puerarin  2,3,5,4'-tetrahydroxystibene-2-O-β-D-glucoside  hyperoside  quercetin  oleanolic acid  MRM

摘要:

目的 建立UHPLC-ESI-MS/MS同时测定心安宁胶囊中葛根素、二苯乙烯苷、金丝桃苷、槲皮素、齐墩果酸的含量。方法 采用InertSustain^® C₁₈色谱柱（3.0 mm×100 mm，3.0 μm），乙腈-0.1%甲酸水溶液，梯度洗脱，流速0.4 mL·min^-1，进样量10 μL；质谱采用电喷雾离子源（ESI源），负离子扫描模式，多重反应监测模式进行定量分析。结果 心安宁胶囊中5种成分在线性范围内峰面积与浓度均呈良好的线性关系，仪器精密度RSD<2.0%，平均加样回收率为99.15%~99.89%，RSD为0.89%~2.21%。在所设定的色谱条件下，心安宁胶囊中葛根素、二苯乙烯苷、金丝桃苷、槲皮素、齐墩果酸5个成分于10 min内完全分离。结论 建立的UHPLC-ESI-MS/MS方法快速简便、精密度好、灵敏度高，可用于心安宁胶囊中多种成分的含量测定和质量控制。

Abstract:

OBJECTIVE To develop a method for simultaneous determination of puerarin, 2,3,5,4'-tetrahydroxystibene-2-O-β-D-glucoside, hyperoside, quercetin and oleanolic acid in Xin'anning capsules by UHPLC-ESI-MS/MS. METHODS The analysis was performed with triple quadrupole mass spectrometer by electrospray ionization(ESI^-)mode and on InertSustain^® C₁₈ chromatographic column(3.0 mm×100 mm, 3.0 μm). The mobile phase was acetonitrile and 0.1% formic acid-water with gradient elution at a flow rate of 0.4 mL·min^-1, and the injection volume was 10 μL. RESULTS For the UHPLC-ESI-MS/MS assay, the calibration curve was linear, the precision of RSD was less than 2.0%, the average recoveries ranged from 99.15% to 99.89%, RSD ranged from 0.89% to 2.21%. And under the optimized chromatographic conditions, the complete separation of 5 target components were obtained within 10 min. CONCLUSION The established UHPLC-ESI-MS/MS can be served as a scientific and effective way for quality control of Xin'anning capsules.