TY - JOUR
T1 - Determination of hydroxy metabolites of polycyclic aromatic hydrocarbons by fully automated solid-phase microextraction derivatization and gas chromatography-mass spectrometry
AU - Luan, Tiangang
AU - Fang, Shenghong
AU - Zhong, Yin
AU - Lin, Li
AU - Chan, Sidney M.N.
AU - Lan, Chongyu
AU - Tam, Nora F.Y.
PY - 2007/11/30
Y1 - 2007/11/30
N2 - 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 μg 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 μg L-1, respectively, while the respective quantification limits were 0.003-0.044, 0.005-0.081 and 0.008-0.447 μg 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.
AB - 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 μg 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 μg L-1, respectively, while the respective quantification limits were 0.003-0.044, 0.005-0.081 and 0.008-0.447 μg 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.
KW - Biodegradation
KW - Metabolites
KW - Microorganisms
KW - Polycyclic aromatic hydrocarbons
KW - Solid-phase microextraction (SPME)
UR - http://www.scopus.com/inward/record.url?scp=35748957195&partnerID=8YFLogxK
U2 - 10.1016/j.chroma.2007.10.038
DO - 10.1016/j.chroma.2007.10.038
M3 - Article
C2 - 17976631
AN - SCOPUS:35748957195
SN - 0021-9673
VL - 1173
SP - 37
EP - 43
JO - Journal of Chromatography A
JF - Journal of Chromatography A
IS - 1-2
ER -