UPLC-MS/MS同时测定腰息痛胶囊中5种成分含量  

Simultaneous Determination of Five Constituents in Yaoxitong Capsules by UPLC-MS/MS

作　　者：武红娜 黄东杰 贾睿琦 张生潭[2] 姚晨 宋忠强 孙泽民 赵庆林 WU Hong-na;HUANG Dong-jie;JIA Rui-qi;ZHANG Sheng-tan;YAO Chen;SONG Zhong-qiang;SUN Ze-min;ZHAO Qing-lin(Cangzhou Institute for Food and Drug Control,Cangzhou 061000,China;Cangzhou Hospital of Integrated Traditional Chinese and Western Medicine,Cangzhou 061001,China)

机构地区：[1]沧州市食品药品检验所,河北沧州061000 [2]河北省沧州中西医结合医院,河北沧州061001

出　　处：《食品与药品》2024年第5期462-467,共6页Food and Drug

基　　金：河北省中医药管理局指令课题项目(编号:2023269)。

摘　　要：目的建立同时测定腰息痛胶囊中5种成分含量的超高液相色谱-串联质谱法(UPLC-MS/MS)。方法采用Endeavorsil C_(18)(50 mm×2.1 mm,1.8μm)色谱柱;流动相为乙腈(A)-0.1%甲酸(B),梯度洗脱;体积流量0.3 ml/min;柱温30°C;进样量5μl;质谱为电喷雾离子源(ESI源),负离子扫描模式,定量采用多重反应监测模式。结果腰息痛胶囊人参皂苷Rb_(1)、Rb_(3)、Rd、Re和人参皂苷Rg1MS图谱与对照品相同;5种成分在各自范围呈良好线性关系(r>0.9931),平均加样回收率96.7%~97.7%,RSD 0.6%~1.7%,5种成分在5 min内可完全分离。结论该方法高效准确、选择性好,可用于腰息痛胶囊中5种活性成分定量研究。Objective To establish a method for the simultaneous determination of 5 components in Yaoxitong Capsules by UPLC-MS/MS method.Methods The analysis was performed on an Endeavorsil C_(18)(50 mm×2.1 mm,1.8μm)column,using tonitrile-0.1%formic acid at a flow rate of 0.3 ml/min as mobile phase of gradient elution.The column temperature was 30℃,and the injection volume was 5μl.For MS,electro-spray ion source and negative ion scanning mode,as well as multiple reaction monitoring mode were adopted.Results The primary and secondary mass spectrograms of ginsenoside Rb_(1),ginsenoside Rb_(3),ginsenoside Rd,ginsenoside Re and ginsenoside Rg1 in Yaoxitong Capsules were consistent with those of reference solution.Five constituents showed good linear relationships within their own ranges(r>0.9931).The average recoveries were 96.7%-97.7%,with RSDs of 0.6%-1.7%.Under the optimized chromatographic conditions,the complete separation of 5 target components were obtained within 5 min.Conclusion The method is efficient,accurate and selective,and can be used for the quantitative research of five active ingredients in Yaoxitong Capsules.

关 键 词：腰息痛胶囊 超高液相色谱-串联质谱法 中西药复方制剂 含量测定 人参皂苷Rb_(1) 

分 类 号：R927[医药卫生—药学]