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目的:建立HPLC-ELSD法测定猪胆粉中甘氨猪去氧胆酸和甘氨鹅去氧胆酸的含量测定方法。方法:猪胆粉甲醇提取液采用Welch Ultimate Plus C18色谱柱(250 mm×4.6 mm,5μm),以乙腈-0.1%甲酸溶液(40∶60)为流动相,流速为1.0 ml·min~(-1),检测器为奥泰ELSD 2000ES,漂移管温度为105℃,氮气流速为每分钟2.5 L。结果:甘氨猪去氧胆酸和甘氨鹅去氧胆酸分别在0.306~4.590μg(r=0.999 5)、0.280~4.194μg(r=0.999 4)范围内呈现良好的线性关系,其平均回收率分别为99.23%,100.37%,RSD分别为2.0%,1.8%(n=9)。结论:该方法结果准确,灵敏度高,重复性好,可用于猪胆粉的质量控制。
OBJECTIVE: To establish a HPLC-ELSD method for the determination of glycine hyodeoxycholic acid and glycochenodeoxycholic acid in porcine bile powder. Methods: The methanol extract of porcine powder was purified on a Welch Ultimate Plus C18 column (250 mm × 4.6 mm, 5 μm) using acetonitrile-0.1% formic acid solution (40:60) as the mobile phase at a flow rate of 1.0 ml · min ~ 1), the detector is Ottawa ELSD 2000ES, the drift tube temperature is 105 ° C, and the nitrogen flow rate is 2.5 L / min. Results: Glycine hyodeoxycholic acid and glycochenodeoxycholic acid showed a good linear relationship in the range of 0.306 ~ 4.590μg (r = 0.999 5) and 0.280 ~ 4.194μg (r = 0.999 4) Rates were 99.23% and 100.37%, respectively, with RSDs of 2.0% and 1.8%, respectively (n = 9). Conclusion: The method is accurate, sensitive and reproducible. It can be used for the quality control of pig gall powder.