Hollow fibre-based liquid-phase microextraction technique combined with gas chromatography–mass spectrometry for the determination of pyrethroid insecticides in water samples

Abstract

A simple, easy-to-use, efficient and environmentally friendly method has been developed for the simultaneous analysis of nine pirethroid pesticides in water samples by the combination of hollow fibre-based liquid-phase microextraction (HF-LPME) and gas chromatography–mass spectrometry (GC/MS). For the developed method, nine pirethroid pesticides (esbiothrin, prallethrin, bifenthrin, tetramethrin, phenothrin, permethrin, cyfluthrin, cypermethrin and deltamethrin) were concentrated and well separated under optimal conditions. Several factors that influence the efficiency of HF-LPME were investigated and optimized by means of experimental design. The proposed method has good linearity in the concentration range of 10–400μgL−1 with correlation coefficients between 0.995 and 0.999. Overall enrichment factors for the optimized method ranged from 139 to 255 times except for cypermethrin and deltamethrin which ranged from 35 to 128. Detection and quantitation limits of the chromatographic method were in the range of 0.002–0.012μgL−1 and 0.003–0.026μgL−1 respectively, with RSD values between 4.2% and 18.4%. The recoveries varied in the range of 69.4%–122.7% except for cypermethrin and deltamethrin (17.5%–64.1%) with relative standard deviations between 1.0% and 24.0% for intra and inter-day experiments at different concentrations (0.1μgL−1, 0.5μgL−1, 1μgL−1). The HF-LPME method optimized was applied to the analysis of three spiked real water samples with good results.