超高效液相色谱-三重四极杆质谱法同时检测人尿中12种单羟基多环芳烃代谢物

建立了高效、准确的同时测定人体尿样中多种多环芳烃代谢物的方法。取10.0 mL尿液，酶解，经固相萃取净化浓缩、0.2 μm滤膜过滤后，以Acquity UPLC^®HSS T3（100 mm×2.1 mm，1.8 μm）为分析柱，甲醇和水为流动相，采用负离子电喷雾多反应监测模式检测样品中多环芳烃代谢物的含量。12种多环芳烃代谢物在0.04~20.0 μg/L范围内线性关系良好，相关系数>0.99，方法检出限为0.01~0.41 μg/L，平均回收率为80.0%~105%，批内RSD为1.21%~9.12%，批间RSD为4.43%~19.7%。应用该方法对淮河流域某区域的100份人体尿样进行了检测，多环芳烃代谢物的检出率为98%。该方法操作简单，灵敏度高，选择性好，可同时检测尿中12种羟基多环芳烃代谢物。

Simultaneous determination of 12 monohydroxylated polycyclic aromatic hydrocarbon metabolites in human urine by ultra-performance liquid chromatography coupled with triple quadrupole mass spectrometry

An efficient and accurate method was developed for the simultaneous determination of 12 monohydroxylated polycyclic aromatic hydrocarbon metabolites in human urine. A 10.0-mL urine sample was hydrolyzed by enzyme and extracted using solid phase extraction. The metabolites were separated on an Acquity UPLC^®HSS T3 column (100 mm×2.1 mm, 1.8 μm) with a mobile phase comprising methanol and water. The analytes were detected by electrospray ionization (ESI)-MS/MS in negative mode and multiple reaction monitoring (MRM) mode. The linear ranges of the 12 metabolites were 0.04-20.0 μg/L with correlation coefficients above 0.99. The detection limits were in the range of 0.01-0.41 μg/L and the recoveries were 80.0%-105%. The intra-group relative standard deviations (RSDs) were less than 9.12% and the inter-group RSDs were less than 19.7%. This method was applied to the analysis of 100 urine samples and the results showed that the method was simple, sensitive and selective.