title: Determination of hydroxy metabolites of polycyclic aromatic hydrocarbons by fully automated solid-phase microextraction derivatization and gas chromatography-mass spectrometry.
abstract: A fully automated sample pretreatment method was developed for the detection of mono and dihydroxy metabolites of polycyclic aromatic hydrocarbons (PAHs) by gas chromatography-mass spectrometry in the selected ion monitoring mode. Direct immersion solid-phase microextraction for the extraction of target compounds and the headspace on-fiber silylation with N,O-bis(trimethylsilyl)trifluoroacetamide were performed automatically by a multipurpose autosampler (MPS2). The operating conditions including extraction time, derivatization time, ionic strength, pH, and incubation temperature were optimized. Calibration responses of nine metabolites of PAHs over a concentration range of 0.1-100 microg L(-1) with a correlation coefficient of 0.999 were obtained. The detection limits of the nine metabolites in mini pore water, minimal salts medium and soil extract culture medium were in the range of 0.001-0.013, 0.002-0.024 and 0.002-0.134 microg L(-1), respectively, while the respective quantification limits were 0.003-0.044, 0.005-0.081 and 0.008-0.447 microg L(-1). The reliability was confirmed by the traditional solid-phase extraction method. The proposed method could be used to analyze the metabolites of PAHs degraded by microorganisms such as algae and to determine the biodegradation pathways of PAHs.
authors.affiliation: State Key Laboratory of Biocontrol, School of Life Sciences, Sun Yat-sen University, Guangzhou 510275, China. cesltg@mail.sysu.edu.cn
authors.forename: Tiangang
authors.initials: T
authors.lastname: Luan
authors.forename: Shenghong
authors.initials: S
authors.lastname: Fang
authors.forename: Yin
authors.initials: Y
authors.lastname: Zhong
authors.forename: Li
authors.initials: L
authors.lastname: Lin
authors.forename: Sidney M N
authors.initials: SM
authors.lastname: Chan
authors.forename: Chongyu
authors.initials: C
authors.lastname: Lan
authors.forename: Nora F Y
authors.initials: NF
authors.lastname: Tam
mesh_terms: D001673:Biodegradation, Environmental; D000460:Chlorophyta / Q000378:metabolism; D008401:Gas Chromatography-Mass Spectrometry / Q000379:methods*; D011084:Polycyclic Aromatic Hydrocarbons / Q000032:analysis* / Q000378:metabolism; D015203:Reproducibility of Results; D052617:Solid Phase Microextraction / Q000379:methods*
chemical_list: D011084:Polycyclic Aromatic Hydrocarbons