UPLC-MS/MS法同时测定益气养血口服液中的5种有效成分  

Simultaneous Determination of Five Effective Components in Yiqiyangxue Oral Liquid by Ultra Performance Liquid Chromatography with Tandem Mass Spectrometry

作　　者：岑卫健[1] 范晓苏[2] 朱平川[1] 覃莎[2] 王锦[2] 

机构地区：[1]广西大学亚热带农业生物资源保护与利用国家重点实验室,南宁530004 [2]广西大学化学化工学院,南宁530004

出　　处：《基因组学与应用生物学》2013年第4期557-561,共5页Genomics and Applied Biology

摘　　要：建立了同时测定益气养血口服液中的淫羊藿苷、黄芪甲苷、黄芪皂苷Ⅱ、五味子醇甲和麦冬皂苷D5种有效成分含量的超高效液相色谱一串联质谱（UPLC．MS／MS）分析方法，用AgilentZorbaxRRHDEclipsePlusC18（50mm×2．1mm,1．8μm）色谱柱，流动相：A相为乙腈溶液，B相为含0．2％甲酸的水溶液，流速为0．35mL／min。在电喷雾电离（ESI）iE离子模式下，采用的是多重反应监测模式（MRM）进行检测。结果表明，黄芪甲苷、黄芪皂苷Ⅱ、淫羊藿苷、五味子醇甲和麦冬皂苷D的线性范围分别为0．003～12mg／L、0.3～12mg／L、0．009～18mg／L、0．006～1．2mg／L、0．003-310mg／L；检出限分别为1μg／L、1μg／L、3μg／L、2μg/L、1μg／L；5种成分的加样回收率为75．9％～1040／0；相对标准偏差均不大于3．8％。该方法简便、准确、快速、高灵敏度，已成功地用于实际的样品分析。A method for the simultaneous determination of icariin, astragaloside IV, astragaloside II, schisandtin and ophiopogonin D in Yiqiyangxue oral liquid was established by ultra performance liquid chromatography with tandem mass spectrometry （UPLC-MS/MS）. The UPLC separation was performed on a Agilent Zorbax RRHD E- clipse Plus C 18 （50 mmx2.1 mm, 1.8 μm） by using 0.2% （V/V） formic acid aqueous solution and acetonitrile as mo- bile phases with the gradient elution at a flow rate of 0.35 mL/min. The analytes were detected by tandem mass spec- trometry under the positive ion mode with the electrospray ionization （ESI） source and in the multiple reaction moni toting （MRM） mode. Under the optimized conditions, the calibration curves were linear in the ranges of 0.009-18 mg/L for icariin, 0.003-12 mg/L for astragaloside IV, 0.3-12 mg/L for astragaloside II, 0.006-1.2 mg/L for schisandrin, 0,003-3.0 mg/L for ophiopogonin D with the detection limits of 1 μg/L, 1 μg/L, 3 μg/L, 2 μg/L, 1 μg/L, respectively. The average recoveries of the five effective components were between 75.9%-104% with the relative standard de- viations not more than 3.8%. The developed method is simple, accurate, rapid and high sensitivity for the quality control of the five effective components in Yiqiyangxue oral liquid.

关 键 词：益气养血口服液 有效成分 超高效液相色谱-串联质谱(UPLC-MS/MS) 

分 类 号：R286.0[医药卫生—中药学]