目的 建立高效液相色谱-质谱法测定人尿液中乙基葡萄糖醛酸苷.方法 取空白人尿液加入EtG-D5内标工作液和冷甲醇(4℃),经涡旋、离心,取上清液于水浴氮气吹干,以沉淀杂质,采用Agilent Zorbax Bonus-RP色谱柱分离,以乙腈:0.1％甲酸水溶液(5:95)为流动相,采用负离子模式质谱检测,在选择离子监测模式下进行定性和定量测定.结果 尿液中EtG在50～5 000ng/mL范围内线性关系良好,检出限为18ng/mL,方法同收率为90.2％～101.7％,相对标准偏差小于10％.结论 所建方法简便,具有较高的同收率和精密度,适用于尿液中EtG的检测.%Objective To establish a HPLC-MS method for the determination of EtG in human urine. Methods Urine samples were spiked with the internal standard solution and 4mL cold methanol. After agitation and centrifugation, the supernatant was evaporated to dryness under nitrogen. The HPLC separation was performed on an Agilent Zorbax Bonus-RP column with acetonitrile/O. 1% formic acid (5/95 v/v) as mobile phase. The identification and quantification were carried out by negative electrospray ionization and selected ion monitoring mode( SIM). Results The linear ranges were from 50 to 5 000 ng/mL and the limits of detection ( LOD) was 18 ng/mL. The recoveries were between 90.2% and 101.7%, with the relative standard deviations no more than 10%. Conclusion This method is proved to be simple and of satisfactory recovery and precision. It can be suitable for the determination of EtG in human urine.
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