TY - JOUR
T1 - Determination of hydroxylated metabolites of polycyclic aromatic hydrocarbons in sediment samples by combining subcritical water extraction and dispersive liquid-liquid microextraction with derivatization
AU - Wang, Xiaowei
AU - Lin, Li
AU - Luan, Tiangang
AU - Yang, Lihua
AU - Tam, Nora F.Y.
N1 - Funding Information:
The financial support from National Natural Science Foundation of China (NSFC, Nos. 20977116 , 21077139 and 21277177), the Fundamental Research Funds for the Central Universities , and the Specialized Research Fund for the Doctoral Program of Higher Education (No. 0090171110041 ) is gratefully acknowledged.
PY - 2012/11/13
Y1 - 2012/11/13
N2 - 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 0.2334μgkg-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.
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 0.2334μgkg-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.
KW - Accelerated solvent extraction
KW - Dispersive liquid-liquid microextraction
KW - Hydroxylated polycyclic aromatic hydrocarbons
KW - Sediment
KW - Subcritical water extraction
UR - http://www.scopus.com/inward/record.url?scp=84868202476&partnerID=8YFLogxK
U2 - 10.1016/j.aca.2012.09.028
DO - 10.1016/j.aca.2012.09.028
M3 - Article
C2 - 23107137
AN - SCOPUS:84868202476
SN - 0003-2670
VL - 753
SP - 57
EP - 63
JO - Analytica Chimica Acta
JF - Analytica Chimica Acta
ER -