LC-MS/MS同时测定芪桂苓合剂中7个成分  

Simultaneous determination of seven components in Qiguiling mixture by LC-MS/MS

作　　者：王博 杨忠杰 裴媛[1] 荣晓哲 刘玉萍 王瑞[1,2,3] WANG Bo;YANG Zhong-jie;PEI Yuan;RONG Xiao-zhe;LIU Yu-ping;WANG Rui(Department of Pharmacy,Luohe Central Hospital,Luohe 462000,China;Henan Provincial Chinese Medicine Key Laboratory of TCM Preparations and Processing,Luohe 462000,China;Henan Engineering Research Center of TCM Preparation Modernization Technology and Clinical Application,Luohe 462000,China)

机构地区：[1]漯河市中心医院药学部,漯河462000 [2]河南省中药制剂与加工中医药重点实验室,漯河462000 [3]河南省中药制剂现代化技术研发与临床应用工程研究中心,漯河462000

出　　处：《药物分析杂志》2022年第12期2202-2209,共8页Chinese Journal of Pharmaceutical Analysis

基　　金：2020年中央引导地方科技发展专项(漯财预指[2020]309号);河南省工程研究中心资助项目(豫发改高技[2019]569号)。

摘　　要：目的:建立UPLC-MS/MS法快速测定芪桂苓合剂中黄芪甲苷、升麻素苷、5-O-甲基维斯阿米醇苷、甘草苷、甘草酸、橙皮苷、柴胡皂苷a的含量。方法:采用Kinetex C_(18) 100A色谱柱(50 mm×2.1 mm,2.6μm);流动相为0.1%甲酸水溶液(A)-5 mmol·L^(-1)乙酸铵甲醇(B),梯度洗脱;流速为0.3 mL·min^(-1)。结果:黄芪甲苷、升麻素苷、5-O-甲基维斯阿米醇苷、甘草苷、甘草酸、橙皮苷、柴胡皂苷a的质量浓度分别在0.09798~4.899、0.03164~1.582、0.03212~1.606、0.052~2.6、0.06075~3.0375、0.30654~15.327、0.024~1.2 mg·L^(-1)内与峰面积线性关系良好,平均加样回收率为95.4%~105.0%。4个批次样品中,7个成分的质量浓度依次为1.0744~1.104、0.2799~0.2887、0.5195~0.5455、0.4378~0.4786、0.5703~0.6543、1.1234~1.3636、0.5673~0.5974 g·L^(-1)。结论:该方法快速、灵敏、准确,可为芪桂苓合剂的质量评价提供参考。Objective:To establish an ultra performance liquid chromatography mass spectrometry(UPLC-MS/MS)method for the rapid determination of astragalosideⅣ,prim-O-glucosylcimifugin,5-O-methylvisammioside,liquiritin,glycyrrhizic acid,hesperidin and saikosaponin a in Qiguiling mixture.Methods:The analysis was perfoemed on Kinetex C_(18) 100A column(50 mm×2.1 mm,2.6μm),and the mobile phase was 0.1%formic acid aqueous solution(A)-5 mmol·L^(-1)ammonium formate methanol(B)in a gradient elution manner,the flow rate was 0.3 mL·min^(-1).Results:The 7 compents of astragalosideⅣ,prim-O-glucosylcimifugin,5-O-methylvisammioside,liquiritin,glycyrrhizic acid,hesperidin and saikosaponin a had good linearrelationships in the range of 0.09798-4.899,0.03164-1.582,0.03212-1.606,0.052-2.6,0.06075-3.0375,0.30654~15.327,0.024~1.2 mg·L^(-1),and the average recoveries were between 95.4%and 105.0%.The contents of 7 components in 4 batches of Qiguiling mixture were 1.0744-1.104,0.2799-0.2887,0.5195-0.5455,0.4378-0.4786,0.5703-0.6543,1.1234-1.3636,0.5673-0.5974 g·L^(-1),respectively.Conclusion:The method is rapid,sensitive and accurate,which can provide a reference for the quality evaluation of Qiguiling mixture.

关 键 词：芪桂苓合剂 皂苷 色原酮 液质联用法 含量测定 中药多成分分析 

分 类 号：R917[医药卫生—药物分析学]