超高效液相色谱-串联质谱法快速测定人体尿液中4种巯基尿酸

Rapid Determination of 4 Mercapturic Acids in Human Urine by UHPLC-MS/MS

1.00mL人体尿液样品经自制的萃取装置萃取后,收集萃取液,采用超高效液相色谱-串联质谱法快速测定萃取液中4种巯基尿酸的含量。以Waters Acquity UPLC^(TM) BEH C_(18)色谱柱为固定相,以不同体积比的0.05%(体积分数)乙酸溶液和甲醇的混合液为流动相进行梯度洗脱,串联质谱分析中采用电喷雾负离子源和多反应监测模式,采用内标法定量。4种巯基尿酸的检出限(3S/N)为0.012～0.082μg·L^(-1),测定下限(10S/N)为0.038～0.270μg·L^(-1)。方法用于人体尿液样品的分析,日内回收率为93.9%～102%,日内相对标准偏差(n=7)为2.0%～3.4%,日间回收率为93.4%～102%,日间相对标准偏差(n=7)为2.4%～4.1%。

The sample of human urine(1.00 mL) was extracted by self-made extraction device.The extract was collected.UHPLC-MS/MS was applied to the rapid determination of 4 mercapturic acids in the extract.Waters Acquity UPLCTM BEH C18 chromatographic column was used as stationary phase,and the mixture of 0.05%(φ) acetic acid solution and methanol mixed in different ratios was used as mobile phase in gradient elution.ESI-and multi-reactions monitor mode were adopted in MS/MS.Internal standard method was used for quantitative.Detection limits(3S/N) and lower limits of determination(10S/N) of the 4 mercapturic acids were in the ranges of 0.012-0.082μg·L-1 and 0.038-0.270μg·L-1 respectively.The proposed method was applied to the analysis of the sample of human urine.Values of recovery and RSDs(n=7) of intra-day were in the ranges of 93.9%-102% and 2.0%-3.4% respectively.Values of recovery and RSDs(n=7) of inter-day were in the ranges of 93.4%-102% and 2.4%-4.1% respectively.