Application of microwave-assisted micellar extraction combined with solid-phase microextraction and high-performance liquid chromatography with UV detection for the determination of organochlorine pesticides in different mud samples

Abstract

An analytical method combining microwave assisted micellar extraction (MAME) followed by solid-phase microextraction (SPME) and high-performance liquid chromatography–ultraviolet high-performance liquid chromatography with UV detection–detection is implemented for the determination of six organochlorine pesticides in different mud samples collected on Gran Canaria Island (Spain). This method allows detection limits to be reduced with respect to MAME extraction and also enables target organochlorine pesticides to be determined in complex matrices due to the clean-up procedure. Several new variables that affect the MAME–SPME process were introduced and optimized. A non-ionic surfactant, polyoxyethylene 10 lauryl ether, and a 60 µm polydimethylsiloxane-divinylbenzene fibre were used for this approach. After systematic investigations, the optimum experimental parameters were fixed. The optimized method provided satisfactory precision (relative standard deviation less than 10%), good recoveries (79.78–117.70%) and detection limits ranging between 28 and 136 ng g−1 for the pesticides studied. The proposed method was successfully applied to the determination of target organochlorine pesticides in several kinds of mud samples of different physico-chemical characteristics and areas. The MAME–SPME method was also validated and applied to a certified reference material.