title: Ultrasound-assisted extraction and solid-phase extraction as a cleanup procedure for organochlorinated pesticides and polychlorinated biphenyls determination in aquatic samples by gas chromatography with electron capture detection.
abstract: The feasibility of developing a quick, easy, efficient procedure for the simultaneous determination of organochlorinated pesticides and polychlorinated biphenyls in aquatic samples using gas chromatography with electron capture detection based on solid-phase extraction was investigated. The extraction solvent (n-hexane/acetone, cyclohexane/ethyl acetate, n-hexane/dichloromethane, n-hexane) for ultrasound-assisted solid-liquid extraction and solid-phase extraction columns (florisil, neutral alumina, acidic alumina, aminopropyl trimethoxy silane, propyl ethylenediamine, aminopropyl trimethoxy silane/propyl ethylenediamine, graphitized carbon black and silica) for cleanup procedure were optimized. The gas chromatography with electron capture detection method was validated in terms of linearity, sensitivity, reproducibility, and recovery. Mean recoveries ranged from 75 to 115% with relative standard deviations <13%. Quantification limits were 0.20-0.40 ng/g for organochlorinated pesticides and polychlorinated biphenyls. The satisfactory data demonstrated the good reproducibility of the method with relative standard deviations lower than 13%. In comparison to other related methods, this method requires less time and solvent and allows for rapid isolation of the target analytes with high selectivity. This method therefore allows for the screening of numerous samples and can also be used for routine analyses.
authors.affiliation: Key Laboratory of Sustainable Utilization of Technology Research for Fishery Resource of Zhejiang Province, Marine Fishery Institute of Zhejiang Province, Zhejiang Zhoushan, China.
authors.forename: Xiumei
authors.initials: X
authors.lastname: Sun
authors.forename: Hongmei
authors.initials: H
authors.lastname: Hu
authors.forename: Zhi
authors.initials: Z
authors.lastname: Zhong
authors.forename: Yanjian
authors.initials: Y
authors.lastname: Jin
authors.forename: Xiaojun
authors.initials: X
authors.lastname: Zhang
authors.forename: Yuanming
authors.initials: Y
authors.lastname: Guo
keywords: Aquatic samples; Gas chromatography with electron capture detection; Organochlorinated pesticides; Polychlorinated biphenyls; Solid-phase extraction