HPCE内标法测定三黄泻心汤3种制备方式样品中盐酸小檗碱的含量的差异

目的]建立三黄泻心汤中盐酸小檗碱含量的毛细管电泳内标测定方法,比较3种三黄泻心汤不同制备方式样品中盐酸小檗碱含量差异。方法]以二苯胍为内标物;熔融石英毛细管柱（50μm×80 cm,有效长度71.7 cm）为分离通道;电泳介质为25 mmol/L的硼砂-乙腈（3∶1,V/,V pH=9.12）;柱温为15℃;检测器为DAD检测器,检测波长为275 nm;分离电压为30 kV;进样压力为：5 kPa,15 s,测定样品中盐酸小檗碱的含量。结果]当二苯胍内标物的浓度为60.10μg/m l时,盐酸小檗碱在6.40~97.28μg/m l范围内线性关系良好,r=0.999 57,加样平均回收率为100.17%,RSD为1.75%;运用该法测定中成药剂,结果配方浸膏中盐酸小檗碱含量明显高于传统汤剂和复方浸膏中的含量。结论]该方法操作简便、快速、准确,重复性好,可作为三黄泻心汤质量检测手段。

Differences of the Contents of Berberine for Three Preparation Methods in Sanhuang Xiexin Decoction by High Performance Capillary Electrophoresis with Internal Standard Method

OBJECTIVE:To establish a method for the determination of berberine for three different formulations in Sanhuang Xiexin decoction by capillary zone electrophoresis and to compare the contents of berberine in the three different formulations.METHODS: Diphenyl guanidine was used as the internal standard with a fused silica capillary(50 μm×80 cm,with effective length of 71.7 cm).The analysis was completed in 25 mmol/L Na2B4O7(pH=9.12)-acetonitrile(3∶1)as running buffer at a capillary temperature of 15 ℃ and a voltage of 30 kV.With the DAD detection,at wavelength of 275 nm,the sample was injected by air pressure injection(5 kPa×15 s).RESULTS:The Concentration of the internal standard diphenyl guanidine was 60.1 μg/ml.The linear responses covered the ranges from 6.4-97.28 μg/ml(r=0.999 57).The average recoveries for berberine was 100.17%(RSD=1.75%).The content of berberine in extract recipe was significantly higher than others by the method.CONCLUSION:The method is simple,rapid,accurate,good in reproducibility and separated with satisfactory results.It can be used for the precise determination of berberine in the three different formulations.