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目的:建立控制局方至宝散中牛黄质量的分析方法,用于制剂中投料所用牛黄的品种及质量监控。方法:采用薄层检查法检测猪去氧胆酸成分;采用薄层扫描法对局方至宝散中牛黄的胆酸含量进行测定,展开剂为环己烷-乙酸乙酯-36%乙酸-甲醇(20∶25∶2∶3)上层溶液,展开2次;薄层板为硅胶G板,显色剂为10%硫酸乙醇溶液(V/V)1,05℃加热至斑点显色清晰;检测波长为460 nm;采用高效液相色谱法对局方至宝散中牛黄的胆红素含量进行测定,色谱柱为Kromasil-C18(150 mm×4.6 mm,5μm)柱,流动相为乙腈-1%冰乙酸溶液(95∶5,V/V),流速为1.0 ml/min,检测波长为450 nm。结果:薄层检查法中,猪去氧胆酸的最低检出量为0.04μg。薄层扫描法中,胆酸线性范围为25.1 mg/ml～502.0 mg/ml,相关系数为0.999,检出限为0.06μg;平均加标回收率为100.8%,RSD为1.64%。高效液相色谱法中,胆红素方法线性范围为1.22 mg/ml～61.0 mg/ml,相关系数为0.9999,检出限为0.002μg;平均加标回收率为99.0%,RSD为1.62%。结论:该法操作简便,结果准确可靠,应用性较广。
OBJECTIVE: To establish a method for the analysis of the quality of benghuang in Fangbao Sanzhong, which is used to control the varieties and quality of bezoar used in the preparation. Methods: The content of hyodeoxycholic acid was detected by TLC. The content of bile acids in bezoar was determined by TLC. The developing solvent was cyclohexane-ethyl acetate-36% acetic acid-methanol ( 20:25:2:3) upper solution, expand 2 times; TLC plate is silica gel G plate, the color reagent is 10% sulfuric acid ethanol solution (V / V) 1,05 ℃ heating to the spot color clear; detection wavelength Was 460 nm. The content of bilirubin in Beifangbao San San was determined by HPLC. The column was Kromasil-C18 (150 mm × 4.6 mm, 5 μm) with a mobile phase of acetonitrile-1% ice Acetic acid solution (95: 5, V / V) at a flow rate of 1.0 ml / min with a detection wavelength of 450 nm. Results: The minimum detectable amount of hyodeoxycholic acid in the TLC was 0.04 μg. In TLCS, the linear range of cholic acid was 25.1 mg / ml ~ 502.0 mg / ml, the correlation coefficient was 0.999, and the detection limit was 0.06 μg. The average recovery was 100.8% and the RSD was 1.64%. In HPLC, the linear range of bilirubin was 1.22 mg / ml ~ 61.0 mg / ml, the correlation coefficient was 0.9999, the detection limit was 0.002 μg. The average recovery was 99.0% and the RSD was 1.62%. Conclusion: The method is simple, accurate and reliable, and has wide applicability.