大活络丸及其同系列品种中牛黄的质量分析研究

Quality analysis of Bovis Calculus in Dahuoluo pills and its homologous series

目的:对大活络丸及其同系列品种中牛黄的质量进行分析研究,增加其中贵细药材牛黄的监控方法,为完善其质量标准、规范生产及加强监管力度提供依据。方法:采用Kromasil C_(18)(4.6 mm×150 mm,5μm)色谱柱,以乙腈-1%醋酸水溶液(95∶5)为流动相,检测波长450 nm,建立大活络丸及其同系列品种中游离胆红素和总胆红素的高效液相色谱测定方法,对其中所含牛黄的各成分指标进行综合分析及制定合理限量,有效评价和控制其中牛黄的质量。结果:大活络丸及其同系列品种中部分样品所含的牛黄中的游离胆红素和总胆红素的含量有很大的不同,可能存在牛黄投料量不足,以人工牛黄或游离胆红素替代牛黄投料的情况。结论:综合分析不同类型胆红素的含量及比例可较好地评价大活络丸及其同系列品种中投料用牛黄的质量。该方法操作简便,质量可控性高,可为其他含牛黄制剂中牛黄的质量评价提供借鉴。

Objective：To develop a method for quality control of Bovis Calculus in Dahuoluo pills and its homologous series so as to monitor precious herb quality in consideration of their curative effect. Methods： Unconjugated and total bilirubin contents in bezoar were determined respectively by eluting on a Kromasil C18 column （ 4.6 mm × 150 mm, 5 μ m ）using an ioscratic mobile phase composed of acetonitrile-1% acetic acid aq. （ 95 ： 5 ） and detected at 450 nm. Content results of different biliribin indexes were comprehensively analyzed and reasonable limits were set up, which were then used for effective evaluation and quality analysis of biliribin. Results： Illegal uses of Boris Calculus Artifactus were found. The quality of Bovis Calculus in Dahuoluo pills and its homologous series differed greatly, as indicated by the obvious difference in unconjugated and total biliribin contents. Conclusion： Quality of Bovis Calculus in Dahuoluo pills and its homologous series was well reflected bycontents of unconjugated and total bilirubin. The method established was easy to operate with high effectiveness in quality control, and is able to provide reference for determination of Bovis Calculus in other Bovis Calculus containing Chinese patent drugs.