PMID- 23107137 OWN - NLM STAT- MEDLINE DCOM- 20130325 LR - 20161125 IS - 1873-4324 (Electronic) IS - 0003-2670 (Linking) VI - 753 DP - 2012 Nov 13 TI - Determination of hydroxylated metabolites of polycyclic aromatic hydrocarbons in sediment samples by combining subcritical water extraction and dispersive liquid-liquid microextraction with derivatization. PG - 57-63 LID - S0003-2670(12)01355-4 [pii] LID - 10.1016/j.aca.2012.09.028 [doi] AB - A sample preparation method for the determination of hydroxylated polycyclic aromatic hydrocarbons (OH-PAHs) in sediment samples was developed using gas chromatography-mass spectrometry (GC-MS). Dispersive liquid-liquid microextraction (DLLME) with derivatization was performed following the subcritical water extraction (SWE) that provided which was provided by accelerated solvent extraction (ASE). Several important parameters that affected both SWE extraction and DLLME, such as the selection of organic modifier, its volume, extraction temperature, extraction pressure and extraction time were also investigated. High sensitivity of the hydroxylated PAHs derivatives by N-(tert-butyldimethylsilyl)-N-methyl-trifluoroacetamide (MTBSTFA) could be achieved with the limits of detection (LODs) ranging from 0.0139 (2-OH-nap) to 0.2334 mug kg(-1) (3-OH-fluo) and the relative standard deviations (RSDs) between 2.81% (2-OH-phe) and 11.07% (1-OH-pyr). Moreover, the proposed method was compared with SWE coupled with solid phase extraction (SPE), and the results showed that ASE-DLLME was more promising with recoveries ranging from 57.63% to 91.07%. The proposed method was then applied to determine the hydroxylated metabolites of phenanthrene in contaminated sediments produced during the degradation by two PAH-degraders isolated from mangrove sediments. CI - Copyright (c) 2012 Elsevier B.V. All rights reserved. FAU - Wang, Xiaowei AU - Wang X AD - MOE Key Laboratory of Aquatic Product Safety, School of Life Sciences, Sun Yat-Sen University, Guangzhou 510275, People's Republic of China. FAU - Lin, Li AU - Lin L FAU - Luan, Tiangang AU - Luan T FAU - Yang, Lihua AU - Yang L FAU - Tam, Nora F Y AU - Tam NF LA - eng PT - Journal Article PT - Research Support, Non-U.S. Gov't DEP - 20121001 PL - Netherlands TA - Anal Chim Acta JT - Analytica chimica acta JID - 0370534 RN - 0 (Acetamides) RN - 0 (Acetonitriles) RN - 0 (Fluoroacetates) RN - 0 (Organosilicon Compounds) RN - 0 (Polycyclic Aromatic Hydrocarbons) RN - 0 (Water Pollutants, Chemical) RN - 059QF0KO0R (Water) RN - 77377-52-7 (N-methyl-N-(tert-butyldimethylsilyl)trifluoroacetamide) RN - Z072SB282N (acetonitrile) SB - IM MH - Acetamides/chemistry MH - Acetonitriles/chemistry MH - Fluoroacetates/chemistry MH - *Gas Chromatography-Mass Spectrometry MH - Geologic Sediments/*chemistry MH - Hydrogen-Ion Concentration MH - Liquid Phase Microextraction MH - Organosilicon Compounds/chemistry MH - Polycyclic Aromatic Hydrocarbons/*analysis/isolation & purification/metabolism MH - Pressure MH - Solid Phase Extraction MH - Temperature MH - Time Factors MH - Water/*chemistry MH - Water Pollutants, Chemical/*analysis/isolation & purification/metabolism EDAT- 2012/10/31 06:00 MHDA- 2013/03/26 06:00 CRDT- 2012/10/31 06:00 PHST- 2012/06/23 00:00 [received] PHST- 2012/09/12 00:00 [revised] PHST- 2012/09/14 00:00 [accepted] PHST- 2012/10/31 06:00 [entrez] PHST- 2012/10/31 06:00 [pubmed] PHST- 2013/03/26 06:00 [medline] AID - S0003-2670(12)01355-4 [pii] AID - 10.1016/j.aca.2012.09.028 [doi] PST - ppublish SO - Anal Chim Acta. 2012 Nov 13;753:57-63. doi: 10.1016/j.aca.2012.09.028. Epub 2012 Oct 1.