论文部分内容阅读
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,方法回收率为90.2%～101.7%,相对标准偏差小于10%。结论所建方法简便,具有较高的回收率和精密度,适用于尿液中EtG的检测。
Objective To establish a method for the determination of ethylglucuronide in human urine by high performance liquid chromatography-mass spectrometry. Methods Blank urine was added into EtG-D5 internal standard working solution and cold methanol (4 ℃), vortexed and centrifuged. The supernatant was dried under nitrogen in water bath to precipitate impurities and purified by Agilent Zorbax Bonus-RP column Separation, acetonitrile: 0.1% formic acid aqueous solution (5:95) as the mobile phase, using negative ion mode mass spectrometry, selective ion monitoring mode for qualitative and quantitative determination. Results The linearity of EtG in urine ranged from 50 to 5 000 ng / mL. The detection limit was 18 ng / mL. The recovery rate was 90.2% ~ 101.7%. The relative standard deviation was less than 10%. Conclusion The method is simple, has high recovery and precision, and is suitable for the detection of EtG in urine.