祛瘀生新胶囊化学成分超高效液相色谱-串联质谱法分析及含量测定

Content Determination and Chemical Constituent Analysis for Quyushengxin Capsules by UPLC-MS/MS

目的建立定性分析祛瘀生新胶囊化学成分的超高效液相色谱-串联质谱(UPLC-MS/MS)法,以及测定士的宁和黄芪甲苷的液相色谱法。方法采用UPLC-MS/MS法定性分析祛瘀生新胶囊的特征化学成分,采用液相色谱法测定士的宁和黄芪甲苷的含量。色谱柱为Accucore AQ C18柱(150 mm×2.1 mm,2.6μm),流动相为0.1%甲酸水溶液-甲醇溶液,采用正离子全扫描模式;液相色谱柱为Welchrom C18柱(250 mm×4.6 mm,5μm),士的宁流动相为乙腈-0.2%磷酸水溶液(15∶85,V/V),黄芪甲苷流动相为乙腈-水(32∶68,V/V),蒸发光散射检测器检测,紫外检测器检测波长为260 nm。结果祛瘀生新胶囊中有23个特征峰,包括士的宁、马钱苷酸、芦丁、黄芪甲苷等。士的宁、黄芪甲苷进样量分别在0.11~1.10μg(r=0.9999)和0.49~4.90μg(r=0.9992)范围内与峰面积线性关系良好;平均加样回收率分别为99.62%和99.44%,RSD分别为1.34%和0.90%(n=6)。结论该方法灵敏度高,重复性好,结果准确,专属性强,可为该制剂的质量标准及药效物质基础研究提供参考。

Objective To qualitatively analyze the characteristic chemical components of Quyushengxin Capsules by ultra high performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS),and to determine the content of the two principal components by liquid chromatography.Methods The analysis was performed on an Accucore AQ C18(150 mm×2.1 mm,2.6μm)column,the mobile phase was 0.1%formic acid aqueous solution-methanol solution,by using positive ion full scanning mode.The liquid chromatography column was Welchrom C18(250 mm×4.6 mm,5μm),and the acetonitrile-0.2%phosphoric acid water(15∶85,V/V)was strychning mobile phase,the detection wavelength of the ultraviolet detector was 260 nm;acetonitrile-water(32∶68,V/V)was the mobile phase of astragalosideⅣ,detected by evaporative light scattering detector.Results Liquid quality analysis showed that there were 23 characteristic peaks in Quyushengxin Capsules,which were strychnine,loganic acid,rutin,astragalosideⅣ.Strychnine and astragalosideⅣshowed good linearity in the range of 0.11-1.10μg(r=0.9999)and 0.49-4.90μg(r=0.9992),respectively.The average recoveries of strychnine and astragalosideⅣwere 99.62%and 99.44%,the RSDs were 1.34%and 0.90%,respectively(n=6).Conclusion This method has high sensitivity,good reproducibility,accurate results,and strong specificity,which can provide reference for the quality standard and basic research of the pharmacodynamic substance of the preparation.