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.