Simultaneous determination of 11 hydroxy-polycyclic aromatic hydrocarbons in urine by LLE and UPLC-MS/MS
Objective To develop a method for simultaneous determination of 11 hydroxy-polycyclic aromatic hydrocarbons(OH-PAHs)in urine by ultra-high performance liquid chromatography tandem with mass spectrometry(UPLC-MS/MS).Methods The u-rine sample was hydrolyzed by β-glucuronidase/arylsulfatase in a water bath at 37℃ under the condition of pH 5.5 for 16 h away from light overnight,then extracted by 3.0 mL n-hexane.The upper organic phase was separated from urine sample by vortex and centrifu-gation.The extraction procedure was repeated twice and the two extracts were combined,and evaporated with nitrogen gas to almost dryness.The residues were re-dissolved in 20％acetonitrile solution,followed by gradient elution and separation by a CORTECS C18 column with 10％isopropanol methanol solution and water as mobile phases.The internal standard method was performed to measure the concentrations of 11 OH-PAHs by UPLC-MS/MS under ESI-mode.Results The method showed good linearity for the 11 OH-PAHs(r>0.997),with detection limits of 0.01-0.10 ng/mL.The inter-day recoveries were 79.8％-97.3％,with relative standard deviations of 1.9％-4.7％(n= 3),and the intra-day recoveries were 78.6％-92.3％,with relative standard deviations of 3.7％-7.1％(n=3).Conclusion The proposed method is sensitive and accurate,and is suitable for the monitoring of multiple OH-PAHs in human urine samples.
ultra-high performance liquid chromatography-tandem with mass spectrometry(UPLC-MS/MS)hydroxy-polycyclic aromatic hydrocarbons(OH-PAHs)liquid-liquid extraction(LLE)urine
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