Kim, Min-Sun Kang, Tae Woo Pyo, Heesoo Yoon, Junheon Choi, Kyunghee Hong, Jongki 2024-01-20T22:32:32Z 2024-01-20T22:32:32Z 2021-09-03 2008-10-24 0021-9673 https://pubs.kist.re.kr/handle/201004/133047 An analytical method for the determination of organochlorine pesticides (OCPs) in sediment samples involves ultrasonic extraction, solid-phase extraction (SPE), gas-chromatography (CC)/electron-capture detection (ECD), and GC/mass spectrometry (MS). OCPs were extracted from sediment samples by ultra-sonication in mixtures of n-hexane and acetone. Several SPE sorbents [Florisil, silica gel, C18, Oasis HLB, and graphitized carbon black (GCB)] were evaluated as means of preliminary purification. GCB SPE cartridges successfully removed major contaminants such as non-polar hydrocarbons when eluted with an acetone-acetonitrile mixture. After purification, the extract was preferentially screened using GC/ECD and confirmed and quantified using CC/MS. The percentage recovery of samples spiked with 10 or 100ng/g OCP ranged from 73.9% to 106.0% with a relative standard deviation of 0.4-5.7%. Detection limits ranged from 0.002 to 0.005 ng/g for GC/ECD and from 0.03 to 0.50 ng/g for GC/MS detection. The linear dynamic range extended from 0.2 to 20 ng/g, with a correlation coefficient (R-2) greater than 0.995. The method was validated using a standard reference material (SRM 1941b) and spiked sediment samples. Real sediment samples collected from a river near a Korean industrial area exhibited low levels of several OCPs when analyzed using this method. (C) 2008 Elsevier B.V. All rights reserved. English ELSEVIER SCIENCE BV PERSISTENT ORGANIC POLLUTANTS PRESSURIZED LIQUID EXTRACTION ULTRASONIC SOLVENT-EXTRACTION MASS-SPECTROMETRY POLYCHLORINATED-BIPHENYLS CHLORINATED PESTICIDES PYRETHROID PESTICIDES CLEANUP CARTRIDGES SOIL SAMPLES CONTAMINATION Determination of organochlorine pesticides in sediment using graphitized carbon black solid-phase extraction and gas chromatography/mass spectrometry Article 10.1016/j.chroma.2008.08.067 1 JOURNAL OF CHROMATOGRAPHY A, v.1208, no.1-2, pp.25 - 33 JOURNAL OF CHROMATOGRAPHY A 1208 1-2 25 33 scie scopus 000260445900004 2-s2.0-53049091394 Biochemical Research Methods Chemistry, Analytical Biochemistry & Molecular Biology Chemistry Article PERSISTENT ORGANIC POLLUTANTS PRESSURIZED LIQUID EXTRACTION ULTRASONIC SOLVENT-EXTRACTION MASS-SPECTROMETRY POLYCHLORINATED-BIPHENYLS CHLORINATED PESTICIDES PYRETHROID PESTICIDES CLEANUP CARTRIDGES SOIL SAMPLES CONTAMINATION Organochlorine pesticides Sediment Graphitized carbon black Solid-phase extraction Method validation GC/ECD GC/MS