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目的建立HPLC-ELSD同时测定6种胆酸类成分的分析方法,并比较两种牛黄中胆酸类成分的含量。方法采用HPLC-ELSD法,以甲醇和0.1%的醋酸水溶液为流动相,梯度洗脱,流速1.0 mL.min-1,漂移管温度85℃,气体流速2.0 L.min-1。结果石胆酸、熊去氧胆酸、猪去氧胆酸、胆酸、鹅去氧胆酸、去氧胆酸线性范围分别为6.05～96.65,5.37～85.85,4.69～75,6.77～108.35,5.32～85,5.42～86.65 mg.L-1;检测限分别为0.75,0.74,0.65,0.63,0.63,1.05 ng.mL-1;加标回收率分别为99.43%,101.2%,100.4%,102.0%,101.7%,100.0%。结论本法操作简便,结果准确,重现性好,可用于牛黄及其各种制剂中胆酸类成分的质量控制。
OBJECTIVE To establish a method for the simultaneous determination of six cholic acids by HPLC-ELSD and to compare the contents of two cholic acids. Methods The HPLC-ELSD method was used. The mobile phase consisted of methanol and 0.1% acetic acid as mobile phase with a gradient of 1.0 mL · min-1, a drift tube temperature of 85 ℃ and a gas flow rate of 2.0 L.min-1. Results The linear ranges of lithocholic acid, ursodeoxycholic acid, hyodeoxycholic acid, cholic acid, chenodeoxycholic acid and deoxycholic acid were 6.05 ~ 96.65, 5.37 ~ 85.85, 4.69 ~ 75, 6.77 ~ 108.35, 5.32 ~ 85,5.42 ~ 86.65 mg.L-1. The detection limits were 0.75,0.74,0.65,0.63,0.63,1.05 ng.mL-1 respectively. The recoveries of spiked samples were 99.43%, 101.2%, 100.4% and 102.0% , 101.7%, 100.0%. Conclusion This method is simple, accurate and reproducible. It can be used for the quality control of bile acids in bezoar and its various preparations.