PMID- 25703003 OWN - NLM STAT- MEDLINE DCOM- 20151130 LR - 20150223 IS - 1873-3573 (Electronic) IS - 0039-9140 (Linking) VI - 136 DP - 2015 May TI - Determination of eight pharmaceuticals in an aqueous sample using automated derivatization solid-phase microextraction combined with gas chromatography-mass spectrometry. PG - 198-203 LID - S0039-9140(15)00035-1 [pii] LID - 10.1016/j.talanta.2014.11.071 [doi] AB - An automated aqueous derivatization solid-phase microextraction (SPME) coupled with a gas chromatography/mass spectrometry (GC/MS) method was developed for simultaneous determination of eight pharmaceuticals in water samples. Dimethyl sulfate and tetrabutylammonium hydrogen sulfate were selected as derivatization and activation reagents for the esterification reaction. An experimental design approach, central composition design (CCD), was employed to investigate and optimize the operative factors influencing the extraction efficiency, including extraction time, extraction temperature and ionic strength. The other parameters such as type of fiber coating, pH and derivatization conditions were also evaluated. SPME was finally carried out in headspace mode at 80 degrees C for 60min with the presence of 3.00g Na2SO4, using a home-made 44mum PDMS fiber. Wide linear ranges and low limits of detection (0.06-1.24ng L(-1)) were obtained under the optimized conditions. The relative standard deviations (RSDs) and recoveries ranged from 0.5% to 12.3% and 85% to 110%, respectively. The proposed method was successfully applied to the analysis of the real surface water samples from the Pearl River Estuary. CI - Copyright (c) 2015 Elsevier B.V. All rights reserved. FAU - Huang, Siming AU - Huang S AD - MOE Key Laboratory of Aquatic Product Safety/KLGHEI of Environment and Energy Chemistry, School of Chemistry and Chemical Engineering, Sun Yat-sen University, Guangzhou 510275, China. FAU - Zhu, Fang AU - Zhu F AD - MOE Key Laboratory of Aquatic Product Safety/KLGHEI of Environment and Energy Chemistry, School of Chemistry and Chemical Engineering, Sun Yat-sen University, Guangzhou 510275, China. FAU - Jiang, Ruifen AU - Jiang R AD - MOE Key Laboratory of Aquatic Product Safety/KLGHEI of Environment and Energy Chemistry, School of Chemistry and Chemical Engineering, Sun Yat-sen University, Guangzhou 510275, China. FAU - Zhou, Shichun AU - Zhou S AD - MOE Key Laboratory of Aquatic Product Safety/KLGHEI of Environment and Energy Chemistry, School of Chemistry and Chemical Engineering, Sun Yat-sen University, Guangzhou 510275, China. FAU - Zhu, Derong AU - Zhu D AD - Department of Pharmaceutical Analysis, Guangdong Medical College, Dongwan 523808, Guangdong, China. FAU - Liu, Hong AU - Liu H AD - MOE Key Laboratory of Aquatic Product Safety/KLGHEI of Environment and Energy Chemistry, School of Chemistry and Chemical Engineering, Sun Yat-sen University, Guangzhou 510275, China. FAU - Ouyang, Gangfeng AU - Ouyang G AD - MOE Key Laboratory of Aquatic Product Safety/KLGHEI of Environment and Energy Chemistry, School of Chemistry and Chemical Engineering, Sun Yat-sen University, Guangzhou 510275, China. Electronic address: cesoygf@mail.sysu.edu.cn. LA - eng PT - Journal Article PT - Research Support, Non-U.S. Gov't DEP - 20150123 PL - Netherlands TA - Talanta JT - Talanta JID - 2984816R RN - 0 (Pharmaceutical Preparations) RN - 0 (Water Pollutants, Chemical) SB - IM MH - China MH - Environmental Monitoring MH - Gas Chromatography-Mass Spectrometry MH - Pharmaceutical Preparations/*analysis MH - Seawater/*analysis MH - Solid Phase Microextraction MH - Water Pollutants, Chemical/*analysis OTO - NOTNLM OT - Automation OT - Central composite design OT - Derivatization OT - Pharmaceutical OT - Solid-phase microextraction OT - The Pearl River Estuary EDAT- 2015/02/24 06:00 MHDA- 2015/12/15 06:00 CRDT- 2015/02/24 06:00 PHST- 2014/09/10 00:00 [received] PHST- 2014/10/25 00:00 [revised] PHST- 2014/11/01 00:00 [accepted] PHST- 2015/02/24 06:00 [entrez] PHST- 2015/02/24 06:00 [pubmed] PHST- 2015/12/15 06:00 [medline] AID - S0039-9140(15)00035-1 [pii] AID - 10.1016/j.talanta.2014.11.071 [doi] PST - ppublish SO - Talanta. 2015 May;136:198-203. doi: 10.1016/j.talanta.2014.11.071. Epub 2015 Jan 23.