An efficient and fast microwave-assisted extraction method developed for the simultaneous determination of 18 organochlorine pesticides in sediment

Abstract

An efficient and fast microwave-assisted extraction (MAE) method followed by gas chromatographic separation with mass spectrometric detection (GC–MS) was developed for the extraction of 18 organochlorine pesticides (OCPs) from sediment. Parameters affecting the MAE procedure such as the type and volume of the extraction solvent, irradiation power, temperature and irradiation time were successfully optimised. Under the optimal conditions, extraction efficiencies in the range of 73.4–119% were obtained with THF–HEX (9:1, v/v) for all OCPs studied. The method was linear over the range of 2.9–5000 ng g−1 with determination coefficients (r2) higher than 0.992 for all analytes. The limits of detection, LODs (S/N = 3), obtained varied from 1.0 to 2.2 ng g−1 and limits of quantification, LOQs (S/N = 10) were between 2.9 and 6.8 ng g−1. The proposed method was successfully applied to the analysis of real sediment samples and acceptable recoveries from 70.1 to 124% with RSDs ≤14.8% were obtained. 10 OCPs were determined below their LOQ and 8 OCPs in the range of 124–2830 ng g−1. The MAE method was compared with Soxhlet, shake flask and ultrasonic solvent extraction techniques. Thus, the MAE–GC–MS method could efficiently be used for selective extraction and quantification of the target analytes from the complex sediment matrices.