超高效液相色谱-串联质谱法同时测定胆酸钠片中8种胆汁酸成分

Simultaneous determination of eight bile acids in Sodium Cholate Tablets by UPLC-MS

目的 建立了胆酸钠片中8种胆汁酸成分的超高效液相色谱-串联飞行时间质谱(UPLC-Q-tof)的测定方法。方法 采用Waters ACQUITY UPLC HSS T3(1.7μm,2.1×150 mm)色谱柱,以0.01%的甲酸水溶液-乙腈-甲醇梯度洗脱,流速0.6 ml/min,进样2μl,采用飞行时间质谱定量分析。结果 8种胆汁酸成分在各自范围内线性关系良好(r≥0.997 6),平均加样回收率90.5%~102.1%,RSD2.5%~3.7%,定量限1.05~10.30 pg。13批次胆酸钠片各种胆汁酸之和为42.0%~67.7%。结论 该方法准确、简便、灵敏,可用于胆汁酸类药物的质量控制。

Objective To establish a ultra-high performance liquid chromatography coupled with time-of-flight mass spectrometry(UPLCQ-tof) method for simultaneous determination of 8 bile acids in sodium cholate tablets.Methods UPLC separation was performed on a Waters ACQUITY UPLC HSS T3 column with gradient eluent consisting water with 0.01%formic acid, acetonitrile and methanol, and the follow rate was 0.6 ml/min and inject volume was 2μl. The quantitative analyze by time-of-flight mass spectrometry.Results Eight constitutes showed good linear relationships within their own ranges(r ≥ 0.997 6), whose average recoveries were 90.5% ~ 102.1% with the RSDs of 2.5% ~ 3.7% and limit of quantification were 1.05 ~ 10.30 pg. The contents of various bile acids in the 13 batches of samples were 42.0% ~ 67.7%. Conclusion This accurate, simple and sensitive method can be used for quality control of drugs of bile acid type.