尿中多环芳烃代谢物的超高效液相色谱-串联质谱测定法

Determination of polycyclic aromatic hydrocarbons metabolites in urine by ultra-performance liquidchromatography tandem mass spectrometry

目的 建立一种尿中12种多环芳烃代谢物的超高效液相色谱-串联质谱测定方法。方法 2022年选取深圳市的健康成人取其尿样经β-葡萄糖醛酸酶水解后,C18固相萃取柱净化富集,氮吹浓缩,经Waters Acquity UPLC HSS T3 C18色谱柱(100 mm×2.1 mm×1.8μm)分离,在选择反应监测模式下使用UPLC-MS/MS进行检测,内标法定量分析。结果 12种多环芳烃代谢物在0.01~200 ng/mL线性范围良好,相关系数均>0.997 0,检出限为0.002~0.041 ng/mL,定量下限为0.007~0.135 ng/mL,样品加标回收率为88.4%~119.2%。方法批内精密度相对标准偏差(relative standard deviations,RSD)为2.8%~10.3%,批间精密度RSD为3.1%~10.7%。结论 该方法操作简便,灵敏度高、精密度高、检出限低,适合用于人体尿液中12种多环芳烃代谢物的测定。

Objective To develop a method for determination of 12 polycyclic aromatic hydrocarbons metabolites in urine by ultraperformance liquid chromatography tandem mass spectrometry.Methods In 2022,the healthy adults from Shenzhen City were selected to collect their urine samples,the samples were hydrolyzesd byβ-glucuronidase,purified and enriched by C18 solid phase extraction cartridges,concentrated by nitrogen blowing,separated by Waters Acquity UPLC HSS T3 C18 column(100 mm×2.1 mm×1.8μm)and finally determined with UPLC-MS/MS under select response monitoring mode,quantified by internal standard method.Results 12 polycyclic aromatic hydrocarbons metabolites have a good linear relationship in range of 0.01-200 ng/mL,the correlation coefficients were above 0.9970.The limits of detection were 0.002-0.041 ng/mL,the lower limits of quantitation were 0.007-0.135 ng/mL,and the sample spiking recovery rates were 88.4%-119.2%.The relative standard deviations(RSD)of intra batch precision were 2.8%-10.3%,and the RSD of inter batch precision were 3.1%-10.7%.Conclusion This method has the advantages of easy operation,high sensitivity,high precision,low detection limit,and it issuitable for the determination of 12 polycyclic aromatic hydrocarbons metabolites in urine.