功劳去火胶囊中多种指标性成分的同时测定

Simultaneous determination of index components in Gonglao Quhuo capsules

目的:建立高效液相色谱法同时测定功劳去火胶囊中栀子苷、黄芩苷、盐酸小檗碱、汉黄芩苷、黄芩素、汉黄芩素6个成分的含量。方法:样品以用50%乙醇回流提取3 h,采用Agilent Durashell RP色谱柱(4.6 mm×250 mm,5μm),以乙腈-0.05 mol·L-1磷酸二氢钾溶液(p H 3.00)为流动相,梯度洗脱,流速1.0m L·min-1,柱温30℃,检测波长254 nm。结果:栀子苷、黄芩苷、盐酸小檗碱、汉黄芩苷、黄芩素、汉黄芩素6个成分的线性范围及相关系数分别为0.002~0.132 mg·m L^-1(r=1.000),0.010~0.623 mg·m L^-1(r=0.9995),0.003~0.178 mg·mL^-1(r=1.000),0.001~0.081 mg·mL^-1(r=0.9995),0.002~0.100 mg·mL^-1(r=1.000),0.001~0.045 mg·mL^-1(r=1.000);其加样回收率在95.5%~104.9%之间,RSD在0.40%~1.7%之间;11批功劳去火胶囊中每粒分别含栀子苷、黄芩苷、盐酸小檗碱、汉黄芩苷、黄芩素、汉黄芩素2.002~3.179、9.054~16.722、2.541~3.723、0.598~1.456、1.521~2.356、0.299~0.532 mg。结论:本研究所建立的含量测定方法重复性好,准确度高,可用于功劳去火胶囊的质量控制。

Objective:To establish a method for simultaneous determination of geniposide,baicalin,berberine hydrochloride,wogonoside,baicalein and wogonin in Gonglao Quhuo capsules.Methods:The sample was extracted with 50%ethanol by refluxing for 3 h.Agilent Durashell RP(4.6 mm×250 mm,5μm)was used as the solid phase.The mobile phase was acetonitrile-0.05 mol·L-1 potassium dihydrogen phosphate solution(adjusted to pH 3.00 with phosphoric acid)with gradient elution.The column temperature was 30℃,the flow rate was 1.0 mL·min-1,and the detection wavelength was 254 nm.Results:The linear ranges of geniposide,baicalin,berberine hydrochloride,wogonoside,baicalein and wogonin were 0.002-0.132 mg·m L^-1(r=1.000),0.010-0.623 mg·m L^-1(r=0.9995),0.003-0.178 mg·mL^-1(r=1.000),0.001-0.081 mg·mL^-1(r=0.9995),0.002-0.100 mg·mL^-1(r=1.000)and 0.001-0.045 mg·mL^-1(r=1.000),respectively.The average recoveries were 95.5%-104.9%with the RSDs within 0.40%-1.7%.The contents of the six components in 11 batches of samples were 2.002-3.179,9.054-16.722,2.541-3.723,0.598-1.456,1.521-2.356 and 0.299-0.532 mg per capsule.Conclusion:The established method for content determination by this research has good reproducibility and high accuracy,and can be used for quality control of Gonglao Quhuo capsules.