Open AccessDetermination of kepone residue in seawater by gas chromatography coupled with electron capture detector
Author(s) -
Yanjie Wang,
Guangshui Na,
Zhen Wang,
Ziwei Yao
Publication year - 2013
Publication title -
sepu/chinese journal of chromatography
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 0.171
H-Index - 19
eISSN - 1872-2059
pISSN - 1000-8713
DOI - 10.3724/sp.j.1123.2012.04013
Subject(s) - seawater , chromatography , chemistry , detection limit , electron capture detector , gas chromatography , sulfuric acid , analyte , extraction (chemistry) , dichloromethane , solvent , elution , sample preparation , methanol , analytical chemistry (journal) , inorganic chemistry , oceanography , organic chemistry , geology
The effects of extraction solvent, capillary column, cleanup method, co-eluted analytes and other influencing factors on the detection of kepone in seawater were investigated. The analytical method of gas chromatography (GC) coupled with electron capture detector (ECD) was established to determine kepone in seawater. In the method, liquid-liquid extraction and sulfuric acid cleanup were used in the sample pre-processing. Chromatographic analysis was performed on a DB-5 capillary column with external standard method. The kepone was extracted from a 1 L seawater sample by 50 mL dichloromethane. Sulfuric acid was used to remove the interference materials co-extracted from the sample. After cleanup, the extract was dissolved in 1% (v/v) methanol/hexane solvent and analyzed by GC-ECD. In the linear range from 5 microg/L to 100 microg/L of kepone, the correlation coefficient was 0.998 9. The average spiked recoveries were 81% - 108% with the relative standard deviations (RSDs) of 1.2% -5.1% (n = 6). The detection limit was 0.6 ng/L. This method shows good extraction efficiency, high sensitivity and good reproducibility, and is suitable for the determination of kepone in seawater.