Determination of organochlorine pesticides in water using microwave assisted headspace solid-phase microextraction and gas chromatography

A coupled technique, microwave-assisted headspace solid-phase microextraction (MA–HS-SPME), was investigated for one-step in situ sample pretreatment for organochlorine pesticides (OCPs) prior to gas chromatographic determination. The OCPs, aldrin, o,p′-DDE, p,p′-DDE, o,p′-DDT, p,p′-DDT, dieldrin, α-endosulfan, β-endosulfan, endosulfan sulfate, endrin, δ-HCH, γ-HCH, heptachlor, heptachlor epoxide, methoxychlor and trifluralin were collected by the proposed method and analyzed by gas chromatography with electron-capture detection (GC–ECD). To perform the MA–HS-SPME, six types of SPME fibers were examined and compared. The parameters affecting the efficiency in MA–HS-SPME process such as sampling time and temperature, microwave irradiation power, desorption temperature and time were studied to obtain the optimal conditions. The method was developed using spiked water samples such as field water and with 0.05% humic acid in a concentration range of 0.05–2.5 μg/l except endosulfan sulfate in 0.25–2.5 μg/l. The detection was linear over the studied concentration range with r2>0.9978. The detection limits varied from 0.002 to 0.070 μg/l based on S/N=3 and the relative standard deviations for repeatability were <15%. A certified reference sample of OCPs in aqueous solution was analyzed by the proposed method and compared with the conventional liquid–liquid extraction procedure. These results are in good agreement. The results indicate that the proposed method provides a very simple, fast, and solvent-free procedure to achieve sample pretreatment prior to the trace-level screening determination of organochloride pesticides by gas chromatography.