西黄丸定性定量方法的研究

目的: 提高、完善西黄丸的质量标准。 方法: 建立处方中乳香、没药的薄层色谱鉴别方法;采用HPLC-ELSD法检查处方中猪去氧胆酸,使用Agilent ZORBAX SB C₁₈(250 mm×4.6 mm,5 μm)色谱柱,以乙腈-0.5%甲酸(38∶ 62)为流动相,流速1.0 mL·min^-1,柱温35 ℃,Alltech 2000ES蒸发光散射检测器(漂移管温度为90 ℃,气体流量2 L·min^-1);采用HPLC法测定牛黄(体外培育牛黄)中胆红素的含量,使用Agilent ZORBAX SB C₁₈(250 mm×4.6 mm,5 μm),以乙腈-1%醋酸溶液(95∶ 5)为流动相,流速1.0 mL·min^-1,检测波长为450 nm,柱温40 ℃。 结果: 薄层色谱斑点清晰,专属性强;HPLC-ELSD检查方法方便、快捷,专属性强;HPLC方法学考察结果表明胆红素浓度在0.0046~0.1145 mg·mL^-1范围内线性关系良好(r=0.9993);平均加样回收率(n=6)为100.6%(RSD=1.8%)。 结论: 建立的方法简便、准确,重复性好,可作为西黄丸的定性定量方法。

Objective: To enhance and consummate the quality standard of Xihuang pills. Methods: Frankincense,myrrh were identified by TLC.Hyodeoxycholic acid in prescription was checked by HPLC-ELSD;The chromatographic column was Agilent ZORBAX SB C₁₈(250 mm×4.6 mm,5 μm),the mobile phase was acetonitrile-0.5% formic acid(38︰62) at the flow rate of 1.0 mL·min^-1,and column temperature was 35 ℃;The flow rate of N₂ in ELSD was 2 L·min^-1,and the temperature of drift tube was 90 ℃.The contents of bilirubinic in bezoar(cultured ox gallstone) were determined by HPLC;The chromatographic column was Agilent ZORBAX SB C₁₈(250 mm×4.6 mm,5 μm),the mobile phase was acetonitrile-1% acetic acid(95∶ 5) at the flow rate of 1.0 mL·min^-1, the detecting wavelength was 450 nm, and column temperature was 40 ℃. Results: The TLC identification was highly specific and spots were clear.The HPLC-ELSD check-up method was convenient and specific.The bilirubin showed a good linear relationship at a rang of 0.0046-0.1145 mg·mL^-1(r=0.9993),and the average recovery(n=6) was 100.6% with RSD of 1.8%. Conclusion: The method established is accurate, simple and reproducible, and can be used for the study of quality and quantity for Xihuang pills.