Validation of a headspace solid-phase microextraction procedure with gas chromatography-electron capture detection of pesticide residues in fruits and vegetables

Headspace solid-phase microextraction (HS-SPME) was evaluated for the determination of pesticide residues in fruits and vegetables by gas chromatography with an electron capture detector (GC-ECD). The fibre used was coated with polydimethylsiloxane (100 mu m thickness) and the analytical conditions employed have been developed and optimised in a previous work [Chai, M. K., Tan, G. H., & Asha, L. (2008). Optimisation of headspace solid-phase microextraction for the determination of pesticide residues in vegetables and fruits. Analytical Sciences, 24 (2), 273-276]. The results show that the HS-SPME procedure gave a better linear range, accuracy, precision, detection and quantification limits and is adequate for analysing pesticide residues in fruits and vegetables. The average recoveries obtained for each pesticide ranged between 71% and 98% at three fortification levels with the relative standard deviation of less than 5%. Repeatability (0.3-3.7%) and intermediate precision (0.8-2.5%) were shown to be satisfactory. The limits of detection (0.01-1 mu g L(-1)) and the limits of quantification (0.05-5 mu g L(-1)) of these pesticides were much lower than the maximum residue levels (MRL), allowed for fruits and vegetables in Malaysia. (C) 2009 Published by Elsevier Ltd.