超高效液相色谱-串联质谱法同时测定胆汁中15种胆汁酸

Simultaneous determination of fifteen bile acids in bile by ultra performance liquid chromatography with tandem mass spectrometry

建立了同时测定胆汁中15种胆汁酸的超高效液相色谱-串联质谱分析方法。以蛋白质沉淀的方法对样品进行前处理。以甲醇和0.1%（V/V）甲酸水为流动相对目标物进行梯度洗脱。在电喷雾负离子模式,采用多反应监测进行定性和定量分析。15种胆汁酸在线性范围内线性关系良好,线性相关系数（R2）均大于0.993;目标物的检出限为0.2~2.0μg/L;3个加标水平下的回收率为71.8%~96.5%,相对标准偏差为2.7%~8.5%。方法可用于胆汁中胆汁酸的检测。

A sensitive method was developed for the simultaneous determination of fifteen bile acids in bile by ultra performance liquid chromatography-tandem mass spectrometry（ UPLC-MS / MS）. Protein precipitation with acetonitrile was used for sample preparation. The separation was performed by using 0. 1 %（ V / V） formic acid water and methanol as the mobile phase with gradient elution. The electrospray ionization（ ESI） source in negative ion mode was used for the analysis of the fifteen bile acids in the multiple reaction monitoring（ MRM）mode. The results verified that the standard curve for each bile acid was obtained with good correlation coefficient（ R2〉 0. 993） in their concentration range. The limits of detection for the fifteen bile acids were in the range of0. 2-2. 0 μg / L. The mean recoveries for the fifteen bile acids were 71. 8% ~ 96. 5% with relative standard deviations of 2. 7% ~ 8. 5%, respectively. The method is accurate, simple, rapid and feasible for the simultaneous determination of bile acids in bile.