title: Determination of eight pharmaceuticals in an aqueous sample using automated derivatization solid-phase microextraction combined with gas chromatography-mass spectrometry.
abstract: 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°C for 60min with the presence of 3.00g Na2SO4, using a home-made 44μm 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.
authors.affiliation: 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.
authors.forename: Siming
authors.initials: S
authors.lastname: Huang
authors.affiliation: 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.
authors.forename: Fang
authors.initials: F
authors.lastname: Zhu
authors.affiliation: 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.
authors.forename: Ruifen
authors.initials: R
authors.lastname: Jiang
authors.affiliation: 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.
authors.forename: Shichun
authors.initials: S
authors.lastname: Zhou
authors.affiliation: Department of Pharmaceutical Analysis, Guangdong Medical College, Dongwan 523808, Guangdong, China.
authors.forename: Derong
authors.initials: D
authors.lastname: Zhu
authors.affiliation: 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.
authors.forename: Hong
authors.initials: H
authors.lastname: Liu
authors.affiliation: 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.
authors.forename: Gangfeng
authors.initials: G
authors.lastname: Ouyang
mesh_terms: D002681:China; D004784:Environmental Monitoring; D008401:Gas Chromatography-Mass Spectrometry; D004364:Pharmaceutical Preparations / Q000032:analysis*; D012623:Seawater / Q000032:analysis*; D052617:Solid Phase Microextraction; D014874:Water Pollutants, Chemical / Q000032:analysis*
chemical_list: D004364:Pharmaceutical Preparations; D014874:Water Pollutants, Chemical
keywords: Automation; Central composite design; Derivatization; Pharmaceutical; Solid-phase microextraction; The Pearl River Estuary