现代中药研究与实践

目的 建立牛黄解毒制剂中9个指标成分的高效液相色谱(HPLC)含量测定方法。方法 采用Xbridge C₁₈色谱柱(4.6 mm × 250 mm，5 μm)；流动相为乙腈-0.1%磷酸水溶液，梯度洗脱；流速为1.30 mL/min；柱温为30 ℃；254和280 nm双波长检测。应用所建立的HPLC方法对市售四种牛黄解毒制剂(丸、片、胶囊和软胶囊)11个厂家样品中9个成分进行含量测定。结果 经方法学验证各项指标均合要求。11个厂家牛黄解毒制剂中9个指标成分含量范围为：黄芩苷6.78 ～ 22.03 mg/g、汉黄芩苷1.52 ～ 5.94 mg/g、黄芩素0.33 ～ 2.72 mg/g、甘草酸0.41 ～ 2.85 mg/g、芦荟大黄素0.06 ～ 0.84 mg/g、大黄酸0.10 ～ 1.07 mg/g、大黄素0.08 ～ 1.24 mg/g、大黄酚0.80 ～ 6.55 mg/g、大黄素甲醚0.10 ～ 0.85 mg/g。结论 所建立的HPLC含量测定方法技术简单、灵敏度高、重复性好，可用于牛黄解毒制剂的质量评价。

Objective To establish a high performance liquid chromatography (HPLC) method for the content determination of 9 indicator components in Niuhuang Jiedu preparations.Methods A Xbridge C₁₈ column (4.6 mm × 250 mm,5 μm) was used;the mobile phase was acetonitrile-0.1% phosphoric acid aqueous solution with gradient elution;the flow rate was 1.30 mL/min;the column temperature was 30 °C;dual-wavelength detection at 254 and 280 nm.The established HPLC method was applied to determine the content of 9 components in commercial Niuhuang Jiedu preparations (pills,tablets,capsules and soft capsules) from 11 manufacturers.Results The validation of the HPLC methodology met all the required indicators.The content range of 9 indicator components in Niuhuang Jiedu preparations from 11 manufacturers was:baicalin 6.78-22.03 mg/g,wogonoside 1.52-5.94 mg/g,baicalein 0.33-2.72 mg/g,glycyrrhizic acid 0.41-2.85 mg/g,aloeemodin 0.06-0.84 mg/g,rhein 0.10-1.07 mg/g,emodin 0.08-1.24 mg/g,chrysophanic acid 0.80-6.55 mg/g and physcion 0.10-0.85 mg/g.Conclusion The established HPLC method for content determination is technically simple,highly sensitive,and has good repeatability,which can be used for the quality evaluation of Niuhuang Jiedu preparations.