高效液相色谱-电化学法测定乙肝舒康胶囊中6种酚酸

HPLC-ECD determination of six phenolic acids in Yiganshukang capsules

目的:建立同时测定乙肝舒康胶囊中没食子酸、原儿茶酸、绿原酸、咖啡酸、香草酸和阿魏酸含量的高效液相色谱-电化学(HPLC-ECD)法。方法:采用 Hypersil ODS(4.6mm×250mm,5.0μm)色谱柱;以甲醇(A)-0.1%醋酸水溶液(pH=3.50)(B)为流动相,梯度洗脱:0min,A-B(2:98);17min,A-B(20:80);30min,A-B(90:10),流速为0.8mL·min^(-1),柱温为30℃,电化学检测器的工作电压为0.7V,采用标准曲线法对6种酚酸进行定量。结果:在选定的色谱条件下没食子酸、原儿茶酸、绿原酸、咖啡酸、香草酸和阿魏酸的检出限分别为1,3,3,6,1,5ng。6种酚酸的平均加样回收率均在98.7%～99.6%之间,RSD 在2.1%～3.2%之间。结论:方法简便、快速、准确,可作为检测乙肝舒康胶囊中酚酸类成分含量的有效方法。

Objective： To establish an HPLC - ECD method for simultaneous determination of the contents of gallic acid, protocatechuic acid, chlorogenic acid, caffeic acid, vanillin acid and ferulic acid in Yiganshukang capsules. Method： The separation was performed on Hypersil ODS （4.6 mm × 250 mm, 5.0 μm） by gradient elution with methanol -0. 1%aqueous acetic acid （ pH = 3.50） （0 min,2： 98; 17 min,20：80;30 min,90： 10） as the mobile phase at a flow rate of 0. 8 mL · min^-1 The detection was done at 0. 7 V and 30 ℃. The samples were filtered through 0. 45 μm membrane. Calibrations of peak area versus concentration were applied in the determination. Resuits：The limits of detection （ng） were 1 for gallic acid,3 for protocatechuic acid,3 for chlorogenic acid,6 for caffeic acid ,1 for vanillin acid and 5 for ferulic acid. The average recoveries of six phenolic acids were between 98.7% -99.6% with RSDs of 2. 1% -3.2%. Conclusion：The method is simple, rapid, reproducible and accurate. It can be used for the routine analysis of the six phenolic acids in Yiganshukang capsules.