SPME and SPE comparative study for coupling with microwave-assisted micellar extraction in the analysis of organochlorine pesticides residues in seaweed samples

Abstract

Solid-phase microextraction (SPME) and solid-phase extraction (SPE) procedures were coupling with microwave-assisted micellar extraction for organochlorine pesticides residues determination in seaweed samples. They were optimized, compared and discussed. Preliminary experiments were performed in order to study experimental conditions for the extraction of pesticides from spiked seaweed samples with microwave-assisted micellar extraction (MAME) using a non-ionic surfactant (Polyoxyethylene 10 Lauryl Ether). After that, SPME and SPE were used to clean-up and preconcentrate MAME extract prior the analysis by liquid chromatography with photodiode array (PDA) detection. Excellent results were obtained for both procedures. Average pesticide recoveries between 80.5 and 104.3% for MAME-SPME and between 73.9 and 111.5% for MAME-SPE were obtained. Relative standard deviations (RSDs) were lower than 10.3% and 5.3% respectively for all recoveries tested, and LOD between 138–348 ng g − 1 for MAME-SPME and 2–38 ng g − 1 for MAME-SPE were obtained. The method was validated using Soxhlet extraction procedure. Both methods were applied to analyse target organochlorine pesticides in several seaweed samples and results were compared. These results show the great possibilities of combining MAME-SPE-HPLC-UV for the analysis of seaweed samples, improving the selectivity and sensitivity in the determination of organochlorine pesticides analysis for this kind of samples.