title: Determination of hydroxylated metabolites of polycyclic aromatic hydrocarbons in sediment samples by combining subcritical water extraction and dispersive liquid-liquid microextraction with derivatization.
abstract: 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 μg 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.
authors.affiliation: MOE Key Laboratory of Aquatic Product Safety, School of Life Sciences, Sun Yat-Sen University, Guangzhou 510275, People's Republic of China.
authors.forename: Xiaowei
authors.initials: X
authors.lastname: Wang
authors.forename: Li
authors.initials: L
authors.lastname: Lin
authors.forename: Tiangang
authors.initials: T
authors.lastname: Luan
authors.forename: Lihua
authors.initials: L
authors.lastname: Yang
authors.forename: Nora F Y
authors.initials: NF
authors.lastname: Tam
mesh_terms: D000081:Acetamides / Q000737:chemistry; D000097:Acetonitriles / Q000737:chemistry; D005463:Fluoroacetates / Q000737:chemistry; D008401:Gas Chromatography-Mass Spectrometry; D019015:Geologic Sediments / Q000737:chemistry*; D006863:Hydrogen-Ion Concentration; D059627:Liquid Phase Microextraction; D017646:Organosilicon Compounds / Q000737:chemistry; D011084:Polycyclic Aromatic Hydrocarbons / Q000032:analysis* / Q000302:isolation & purification / Q000378:metabolism; D011312:Pressure; D052616:Solid Phase Extraction; D013696:Temperature; D013997:Time Factors; D014867:Water / Q000737:chemistry*; D014874:Water Pollutants, Chemical / Q000032:analysis* / Q000302:isolation & purification / Q000378:metabolism
chemical_list: D000081:Acetamides; D000097:Acetonitriles; D005463:Fluoroacetates; D017646:Organosilicon Compounds; D011084:Polycyclic Aromatic Hydrocarbons; D014874:Water Pollutants, Chemical; D014867:Water; C059151:N-methyl-N-(tert-butyldimethylsilyl)trifluoroacetamide; C032159:acetonitrile