title: QuEChERS followed by dispersive liquid-liquid microextraction based on solidification of floating organic droplet method for organochlorine pesticides analysis in fish.
abstract: A fast, sensitive and environmental-friendly method was developed to determine 13 organochlorine pesticides in fish tissue through gas chromatography with electron capture detection. Sample was extracted initially by acetonitrile and then concentrated through dispersive liquid-liquid microextraction based on solidification of floating organic droplet (DLLME-SFO). Dispersive solid phase extraction (d-SPE) was not a separate step but integrated to DLLME-SFO procedure. In order to separate the d-SPE sorbent, water and organic phase well, a modification to the glass centrifuge tube was made to achieving high centrifugal speed. The optimized method was validated with recoveries ranging from 88.1% to 121.2% (with relative standard deviations <15%) at three spiked levels for all of the pesticides. Good linearity was achieved at seven concentration levels from 6.25 to 625μgL-1, which corresponded to 0.001-0.100mgkg-1in the sample. The limits of quantification and the limits of detection for 13 OCPs ranged from 1.94×10-3to 4.93×10-3mgkg-1and 6.50×10-4to 1.58×10-3mgkg-1, respectively. The method was successfully applied to analyze real fish samples.
authors.affiliation: Center for Environment and Water Resources, College of Chemistry and Chemical Engineering, Central South University, No. 932 Lushan Nan Road, Yuelu District, Changsha 410083, PR China.
authors.forename: Xiao-Chen
authors.initials: XC
authors.lastname: Wang
authors.affiliation: Center for Environment and Water Resources, College of Chemistry and Chemical Engineering, Central South University, No. 932 Lushan Nan Road, Yuelu District, Changsha 410083, PR China.
authors.forename: Bin
authors.initials: B
authors.lastname: Shu
authors.affiliation: Center for Environment and Water Resources, College of Chemistry and Chemical Engineering, Central South University, No. 932 Lushan Nan Road, Yuelu District, Changsha 410083, PR China.
authors.forename: Shan
authors.initials: S
authors.lastname: Li
authors.affiliation: Center for Environment and Water Resources, College of Chemistry and Chemical Engineering, Central South University, No. 932 Lushan Nan Road, Yuelu District, Changsha 410083, PR China.
authors.forename: Zhao-Guang
authors.initials: ZG
authors.lastname: Yang
authors.affiliation: Center for Environment and Water Resources, College of Chemistry and Chemical Engineering, Central South University, No. 932 Lushan Nan Road, Yuelu District, Changsha 410083, PR China. Electronic address: qiubo1983@csu.edu.cn.
authors.forename: Bo
authors.initials: B
authors.lastname: Qiu
mesh_terms: D000097:Acetonitriles / Q000737:chemistry; D000818:Animals; D005399:Fishes; D006843:Hydrocarbons, Chlorinated / Q000032:analysis*; D059627:Liquid Phase Microextraction / Q000379:methods*; D010575:Pesticides / Q000032:analysis*; D015203:Reproducibility of Results; D052616:Solid Phase Extraction / Q000379:methods; D014874:Water Pollutants, Chemical / Q000032:analysis*
chemical_list: D000097:Acetonitriles; D006843:Hydrocarbons, Chlorinated; D010575:Pesticides; D014874:Water Pollutants, Chemical; C032159:acetonitrile
keywords: Dispersive liquid–liquid microextraction based on solidification of floating organic droplet; Fish; Gas chromatography with electron capture detection; Organochlorine pesticides; QuEChERS