Simultaneous Determination of 7 Hydroxyl Polycyclic Aromatic Hydrocarbons in Urine by Ultrahigh Performance Liquid Chromatography-Tandem Mass Spectrometry with Solid Supported Liquid-Liquid Extraction
An ultrahigh performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS) with solid supported liquid-liquid extraction(SLE) was developed for the determination of seven hydroxyl polycyclic aromatic hydrocarbons(OH-PAHs) in urine samples.08 mL enzymatic hydrolyzed urine sample was extracted on a SLE cartridge.Parameters for SLE
including type and volume of eluting solvent
and nitrogen evaporation pressure were optimized.The adsorbed analytes were eluted with 6 mL ethyl acetate
and the collected eluate was evaporated to dryness under nitrogen at a pressure of 48 kPa at 25 ℃
then analyzed by UPLC-MS/MS and quantified by the internal standard method.Under the optimized conditions
the calibration curves for the analytes were linear in the range of 0.3-3 000 mg·L-1
with correlation coefficients not less than 0.995 1.The detection limits(S/N=3) and quantitation limits(S/N=10) were in the ranges of 0.05-1.0 mg·L-1 and 0.15-3.0 mg·L-1
respectively.The recoveries for OH-PAHs in urine samples at three spiked levels ranged from 70.8% to 117%
with the intra day(n=3) and inter-day(n=3) RSDs of 3.7%-9.6% and 3.7%-11%
respectively.The proposed method was successfully applied in the determination of OH-PAHs in urine from 10 petroleum workers and 10 control groups(college students).Except 2-hydroxy phenanthrene and 9-hydroxy-phenanthrene
the concentrations of the other five OH-PAHs in the urine samples of petroleum workers were much higher than that in the control samples(p<0.05).The proposed SLE method only included two steps
therefore
the proposed method is applicable for the facile and efficient monitoring of OH-PAHs in urine samples.