PMID- 25732691 OWN - NLM STAT- MEDLINE DCOM- 20151113 LR - 20210209 IS - 1873-4324 (Electronic) IS - 0003-2670 (Linking) VI - 866 DP - 2015 Mar 25 TI - Determination of 13 endocrine disrupting chemicals in sediments by gas chromatography-mass spectrometry using subcritical water extraction coupled with dispersed liquid-liquid microextraction and derivatization. PG - 41-47 LID - S0003-2670(15)00187-7 [pii] LID - 10.1016/j.aca.2015.02.011 [doi] AB - In this study, a sample pretreatment method was developed for the determination of 13 endocrine disrupting chemicals (EDCs) in sediment samples based on the combination of subcritical water extraction (SWE) and dispersed liquid-liquid microextraction (DLLME). The subcritical water that provided by accelerated solvent extractor (ASE) was the sample solution (water) for the following DLLME and the soluble organic modifier that spiked in the subcritical water was also used as the disperser solvent for DLLME in succession. Thus, several important parameters that affected both SWE and DLLME were investigated, such as the extraction solvent for DLLME (chlorobenzene), extraction time for DLLME (30s), selection of organic modifier for SWE (acetone), volume of organic modifier (10%) and extraction temperature for SWE (150 degrees C). In addition, good chromatographic behavior was achieved for GC-MS after derivatisation by using N,O-bis(trimethylsilyl) trifluoroacetamide (BSTFA). As a result, proposed method sensitive and reliable with the limits of detection (LODs) ranging from 0.006 ng g(-1) (BPA) to 0.639 ng g(-1) (19-norethisterone) and the relative standard deviations (RSDs) between 1.5% (E2) and 15.0% (DES). Moreover, the proposed method was compared with direct ASE extraction that reported previously, and the results showed that SWE-DLLME was more promising with recoveries ranging from 42.3% (dienestrol) to 131.3% (4,5alpha-dihydrotestosterone), except for diethylstilbestrol (15.0%) and nonylphenols (29.8%). The proposed method was then successfully applied to determine 13 EDCs sediment of Humen outlet of the Pearl River, 12 of target compounds could be detected, and 10 could be quantitative analysis with the total concentration being 39.6 ng g(-1), and which indicated that the sediment of Humen outlet was heavily contaminated by EDCs. CI - Copyright (c) 2015 Elsevier B.V. All rights reserved. FAU - Yuan, Ke AU - Yuan K AD - MOE Key Laboratory of Aquatic Product Safety, School of Life Sciences, Sun Yat-Sen University, Guangzhou 510275, PR China. FAU - Kang, Haining AU - Kang H AD - Shenzhen Entry-Exit Inspection and Quarantine Bureau, Shenzhen 518045, PR China. FAU - Yue, Zhenfeng AU - Yue Z AD - Shenzhen Entry-Exit Inspection and Quarantine Bureau, Shenzhen 518045, PR China. FAU - Yang, Lihua AU - Yang L AD - Guangdong Provincial Key Laboratory of Marine Resources and Coastal Engineering, School of Marine Sciences, Sun Yat-Sen University, Guangzhou 510275, PR China. FAU - Lin, Li AU - Lin L AD - MOE Key Laboratory of Aquatic Product Safety, School of Life Sciences, Sun Yat-Sen University, Guangzhou 510275, PR China. FAU - Wang, Xiaowei AU - Wang X AD - Guangdong Provincial Key Laboratory of Marine Resources and Coastal Engineering, School of Marine Sciences, Sun Yat-Sen University, Guangzhou 510275, PR China. Electronic address: wangxw5@mail.sysu.edu.cn. FAU - Luan, Tiangang AU - Luan T AD - MOE Key Laboratory of Aquatic Product Safety, School of Life Sciences, Sun Yat-Sen University, Guangzhou 510275, PR China. LA - eng PT - Journal Article PT - Research Support, Non-U.S. Gov't DEP - 20150210 PL - Netherlands TA - Anal Chim Acta JT - Analytica chimica acta JID - 0370534 RN - 0 (Acetamides) RN - 0 (Endocrine Disruptors) RN - 0 (N,O-bis(trimethylsilyl)trifluoroacetamide) RN - 0 (Trimethylsilyl Compounds) RN - 059QF0KO0R (Water) SB - IM MH - Acetamides/chemistry MH - Endocrine Disruptors/*analysis/chemistry/isolation & purification MH - *Gas Chromatography-Mass Spectrometry MH - Geologic Sediments/*chemistry MH - Liquid Phase Microextraction MH - Temperature MH - Trimethylsilyl Compounds/chemistry MH - Water/chemistry OTO - NOTNLM OT - Derivatization OT - Dispersed liquid-liquid extraction OT - Endocrine disrupting chemicals OT - Sediment OT - Subcritical water extraction EDAT- 2015/03/04 06:00 MHDA- 2015/11/14 06:00 CRDT- 2015/03/04 06:00 PHST- 2014/10/03 00:00 [received] PHST- 2015/01/29 00:00 [revised] PHST- 2015/02/08 00:00 [accepted] PHST- 2015/03/04 06:00 [entrez] PHST- 2015/03/04 06:00 [pubmed] PHST- 2015/11/14 06:00 [medline] AID - S0003-2670(15)00187-7 [pii] AID - 10.1016/j.aca.2015.02.011 [doi] PST - ppublish SO - Anal Chim Acta. 2015 Mar 25;866:41-47. doi: 10.1016/j.aca.2015.02.011. Epub 2015 Feb 10.