HPLC-CAD法同时测定腰痹通胶囊中5种皂苷含量

Simultaneous determination of five saponins in Yaobitong capsule by HPLC-CAD

建立了高效液相色谱法联合电雾式检测器(charged aerosol detector,CAD)同时测定腰痹通胶囊中5种皂苷(三七皂苷R1、人参皂苷Rg1、人参皂苷Re、人参皂苷Rb1、人参皂苷Rd)含量,为腰痹通胶囊的质量控制提供了方法依据。以甲醇提取样品,色谱柱为Waters XBridge Phenol(150 mm×4.6 mm,3.5μm),以乙腈-水为流动相进行梯度洗脱,柱温为30℃,流速为1.0 mL·min^-1,进样量为10μL。电雾式检测器的雾化温度为35℃,气压为60.2 psi,滤波为3.6 s,采集频率为5 Hz。三七皂苷R1、人参皂苷Rg1、人参皂苷Re、人参皂苷Rb1、人参皂苷Rd的线性关系良好,线性范围分别为16.96~203.5μg·mL^-1(R2=0.9993)、54.46~653.5μg·mL^-1(R2=0.9993)、10.96~131.5μg·mL^-1(R^2=0.9996)、51.50~618.0μg·mL^-1(R^2=0.9990)、15.94~191.3μg·mL-1(R^2=0.9994),平均回收率分别为98.96%、100.8%、94.76%、100.1%、103.1%,RSD分别为0.87%、1.46%、1.85%、2.06%、0.96%(n=6)。结果表明,此方法准确、简便、可靠,可用于腰痹通胶囊中5种皂苷的含量测定。

A high performance liquid chromatography charged aerosol detector(HPLC-CAD)method was established for the simultaneous determination of five saponins(notoginsenoside R1,ginsenoside Rg1,ginsenoside Re,ginsenoside Rb1,Ginsenoside Rd)in Yaobitong capsule,providing a method for quality control.The sample was extracted with methanol and chromatographic separation was performed on a Waters Xbridge Phenol column(150 mm×4.6 mm,3.5μm)using acetonitrile-water as the mobile phase with gradient elution at a flow rate of1.0 mL·min-1.The column temperature was 30℃and the injection volume was 10μL.The nebulizer temperature of CAD was 35℃and the air pressure was 60.2 psi,the filtration was 3.6 s,and the collection frequency was5 Hz.Notoginsenoside R1,ginsenoside Rg1,ginsenoside Re,ginsenoside Rb1 and ginsenoside Rd showed a good linear relationship in the range of 16.96-203.5μg·mL-1(R^2=0.9993),54.46-653.5μg·mL-1(R2=0.9993),10.96-131.5μg·mL^-1(R^2=0.9996),51.50-618.0μg·mL^-1(R^2=0.9990),15.94-191.3μg·mL-1(R^2=0.9994),respectively The average recoveries were 98.96%,100.8%,94.76%,100.1%,103.1%,and RSDs were 0.87%,1.46%,1.85%2.06%,0.96%(n=6),respectively.The proposed method is accurate,simple and reliable,and can be used for the determination of five saponins in Yaobitong capsule.