UPLC-MS/MS法测定心可舒胶囊中5种皂苷类成分的含量

目的:采用超高效液相色谱-串联质谱法建立心可舒胶囊中三七主要成分三七皂苷R₁、人参皂苷Rg₁、人参皂苷Re、人参皂苷Rb₁和人参皂苷Rd的含量。方法:供试品溶液用微波萃取方式制备,用Waters ACQUITY BEH C₁₈(2.1 mm×50 mm,1.7μm)色谱柱,以乙腈和水梯度洗脱为流动相,流速为0.4 mL·min^-1,柱温40℃,电喷雾电离源(ESI),多反应离子监测(MRM)扫描方式进行检测。结果:三七皂苷R₁、人参皂苷Rg₁、人参皂苷Re、人参皂苷Rb₁和人参皂苷Rd质量浓度在0.05~50 ng·mL^-1的范围内线性关系良好(r>0.999),3种浓度水平平均加样回收率分别在92.2%~98.1%、98.4%~101.2%、90.5%~99.6%、90.4%~95.7%和90.2%~91.8%范围内。样品中5种成分含量分别为2.67~229.33、3.33~320.33、1.33~93.33、5.33~446.5和5.61~391.16μg·g^-1。结论:所建立的方法简便灵敏,重复性好,可用于心可舒胶囊中三七的质量控制。

Objective: To establish the method for determination of notoginsenoside R₁, gensenoside Rg₁, gensenoside Re, gensenoside Rb₁ and gensenoside Rd in Xinkeshu capsules by UPLC-MS/MS.Methods: The samples were abstracted by microwave-assisted extraction and were separated on the Waters ACQUITY BEH C₁₈ column(2.1 mm×50 mm, 1.7μm), and eluted with a gradient elution of acetonitrile and water.The flow rate was 0.4 mL·min^-1, and the column temperature was 40℃.The analytes were detected by tandem mass spectrometry with the electrospray ionization(ESI) source combined with multiple reaction monitoring(MRM) mode.Results: The method showed a good linearity in the range of 0.05-50 ng·mL^-1, with the correlation coefficient above 0.999.The recoveries on three concentration levels of notoginsenoside R₁, gensenoside Rg₁, gensenoside Re, gensenoside Rb₁ and gensenoside Rd were 92.2%-98.1%, 98.4%-101.2%, 90.5%-99.6%, 90.4%-95.7% and 90.2%-91.8%.The contents of five components in samples were 2.67-229.33μg·g^-1, 3.33-320.33μg·g^-1, 1.33-93.33μg·g^-1, 5.33-446.5μg·g^-1 and 5.61-391.16μg·g^-1, respectively.Conclusion: The method is simple, sensitive and well repeatable, which can be used for quality control of Xinkeshu capsules.