Simultaneous Determination of 7 Hydroxyl Polycyclic Aromatic Hydrocarbons in Urine by Ultrahigh Performance Liquid Chromatography-Tandem Mass Spectrometry with Solid Supported Liquid-Liquid Extraction
  
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KeyWord:hydroxyl polycyclic aromatic hydrocarbons(OH-PAHs)  solid supported liquid-liquid extraction(SLE)  ultrahigh performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS)  urine
  
AuthorInstitution
CHEN Xue-lei,LI Dong-mei,XU Hou-jun,WANG Xue-sheng,WANG Man-man 1.School of Public Health,North China University of Science and Technology;2.College of Pharmacy,North China University of Science and Technology
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Abstract:
      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.08 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.
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