title: Quantitative determination of organochlorine pesticides in sewage sludges using soxtec, soxhlet and pressurized liquid extractions and ion trap mass-mass spectrometric detection.
abstract: A new analytical method is described for the determination of organochlorine pesticides (OCPs) in sewage sludges using GC-ion trap-MS-MS. In this work, 16 organo-chlorine pesticides (OCPs) listed by the US Environmental Protection Agency (US EPA) as priority pollutants were separated and quantified. Sludge samples from three of Kuwait's wastewater treatment plants (WWTPs) were analyzed for organochlorine pesticides (OCPs). Spiked sludge samples were extracted with a mixture of (1:1 v/v) dichloromethane (DCM)/hexane. The extracts were cleaned on a silica/aluminum oxide column, then transferred to a gel permeation chromatography (GPC) column, before undergoing further silica/aluminum oxide clean-up; the presence of OCPs was then confirmed by GC-ion trap-MS-MS. Three extraction techniques, soxtec, soxhlet, and pressurized liquid extractions were utilized, compared and validated using the spiked sludge samples. The methods were validated in term of accuracy (recovery) and precision (RSD). The method recovery values varied from 76.1 to 92.9% for the three extraction techniques.
authors.affiliation: Central Analytical Laboratory (CAL), Kuwait Institute for Scientific Research (KISR), PO Box 24885, Safat 13109, Kuwait. mrhelaleh@safat.kisr.edu.kw
authors.forename: M I H
authors.initials: MI
authors.lastname: Helaleh
authors.forename: A
authors.initials: A
authors.lastname: Al-Omair
authors.forename: N
authors.initials: N
authors.lastname: Ahmed
authors.forename: B
authors.initials: B
authors.lastname: Gevao
mesh_terms: D000537:Aluminum Oxide / Q000737:chemistry; D005591:Chemical Fractionation / Q000379:methods*; D002849:Chromatography, Gas / Q000295:instrumentation / Q000379:methods; D002850:Chromatography, Gel / Q000379:methods; D006586:Hexanes / Q000737:chemistry; D006843:Hydrocarbons, Chlorinated / Q000032:analysis*; D008752:Methylene Chloride / Q000737:chemistry; D010575:Pesticides / Q000032:analysis*; D010936:Plant Extracts / Q000302:isolation & purification*; D012680:Sensitivity and Specificity; D012822:Silicon Dioxide / Q000737:chemistry; D053719:Tandem Mass Spectrometry / Q000295:instrumentation / Q000379:methods*
chemical_list: D006586:Hexanes; D006843:Hydrocarbons, Chlorinated; D010575:Pesticides; D010936:Plant Extracts; D008752:Methylene Chloride; D012822:Silicon Dioxide; D000537:Aluminum Oxide