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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
Author(s) -
Sun Xiumei,
Hu Hongmei,
Zhong Zhi,
Jin Yanjian,
Zhang Xiaojun,
Guo Yuanming
Publication year - 2015
Publication title -
journal of separation science
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 0.72
H-Index - 102
eISSN - 1615-9314
pISSN - 1615-9306
DOI - 10.1002/jssc.201400880
Subject(s) - chemistry , chromatography , solid phase extraction , extraction (chemistry) , gas chromatography , detection limit , electron capture detector , ethyl acetate , solvent , sample preparation , organic chemistry
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.