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目的建立HPLC-ELSD法同时测定猪胆粉中猪去氧胆酸和鹅去氧胆酸的含量测定方法。方法应用Wa-ters Symmetry C18(4.6 mm×150 mm,5μm)色谱柱,甲醇-0.2%甲酸溶液(80∶20)为流动相,流速:1.0 mL.min-1;柱温:40℃;检测器为ELSD,漂移管温度:85℃,载气为高纯氮气,流量:2.0 L.min-1。结果猪去氧胆酸在0.5192μg～5.1920μg范围内呈良好的线性关系(r=0.999 4),平均加样回收率为97.5%,RSD=2.3%;鹅去氧胆酸在0.5012μg～5.0120μg范围内呈良好的线性关系(r=0.999 8),平均加样回收率为96.0%,RSD=1.6%。结论该方法简便准确,灵敏度高,可用于猪胆粉的质量控制。
OBJECTIVE To establish a HPLC-ELSD method for simultaneous determination of hyodeoxycholic acid and chenodeoxycholic acid in porcine bile powder. Methods The mobile phase consisted of methanol-0.2% formic acid solution (80:20) and a flow rate of 1.0 mL · min-1 at a temperature of 40 ℃ on a Wa-ters Symmetry C18 column (4.6 mm × 150 mm, ELSD device, the drift tube temperature: 85 ℃, carrier gas is high purity nitrogen, flow rate: 2.0 L.min-1. Results Hyodeoxycholic acid had a good linear relationship (r = 0.999 4) in the range of 0.5192μg ~ 5.1920μg, with an average recovery of 97.5% and a RSD of 2.3%, and that of chenodeoxycholic acid was in the range of 0.5012μg ~ 5.0120μg There was a good linear relationship (r = 0.999 8) with an average recovery of 96.0% and RSD of 1.6%. Conclusion The method is simple, accurate and sensitive and can be used for the quality control of porcine bile powder.