3种牛黄及安宫牛黄丸中总胆红素含量测定方法的优化

目的：优化3种牛黄及安宫牛黄丸中总胆红素的含量测定方法。方法：采用10%草酸溶液为牛黄中胆红素的提取溶剂，高效液相色谱法测定总胆红素的含量。为控制牛黄及其制剂的质量提供了依据和方法。色谱柱为迪马Kromasil 100Å C₁₈（5 μm，0.46 mm×150 mm），乙腈-1%醋酸（95：5）为流动相，等度洗脱，检测波长450 nm，柱温30 ℃。结果：在3.63~51.80 μg·mL^-1，胆红素线性相关系数为0.9999，3种牛黄及安宫牛黄丸的加样回收率均在98.0%~105.0%。结论：方法重复性好，准确度较高，能有效提取出样品中的胆红素，避免了牛黄种类不同而导致胆红素提取不完全的问题，。方法操作简便易行，通用性较好，为其他含牛黄类中成药中胆红素的测定提供了参考。

Objective: To establish an optimized method for the determination of total bilirubin in three kinds of Bovis Calculus and Angong Niuhuang pills. Methods: The 10%oxalic acid solution was used as the extraction solvent for the first time.The HPLC separation was performed on a Kromasil 100Å C₁₈ column(5 μm,0.46 mm×150 mm)by using acetonitrile-1%acetic acid(95:5)as the mobile phase for isocratic elution at a flow rate of 1 mL·min^-1at a column temperature of 30 ℃.Samples were detected by UV-VIS detector at 450 nm. Results: Results showed that the optimized method was good at detecting total bilirubin in samples.The correlation coefficient was 0.9999 and the linear relationship was good in the range of 3.63-51.80 μg·mL^-1.After the optimization,recoveries of three kinds of Bovis Calculus and Angong Niuhuang pills were between 98.0%and 105.0%. Conclusion: The method established is reliable and accurate for the analysis of total bilirubin in Bovis Calculus and Angong Niuhuang pills which can avoid the problem of incomplete extraction of bilirubin due to different varieties of Bovis Calculus.The method is simple,convenient,universal,and easy to perform,providing references for determination of bilirubin in other Bovis Calculus containing Chinese patent drugs.

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