A microchip device based liquid-liquid-solid microextraction for the determination of permethrin and cypermethrin in water samples

In this work, for the first time, a microchip device integrating liquid-liquid-solid phase microextraction is presented. As a novel approach to microchip systems, liquid-liquid-solid microextraction was performed in a sandwiched microchip device. The microchip device consisted of three poly(methyl methacrylate) layers along with a double Y-shaped microchannel. As the stationary phase, polyacrylonitrile-C18 was synthesized and immobilized in the upper channel, while the beneath channel was used as a reservoir for the stagnant volume ratio of sample-to-extraction solvent phase. In this way, analytes were extracted from an aqueous sample through an organic phase into the stationary phase. The analytes were finally desorbed with a minimum amount of acetonitrile as the desorption solvent. Permethrin and cypermethrin were selected as the model analytes for extraction and subsequent analysis by gas chromatography-flame ionization detection. Under optimum conditions (extraction solvent; n-hexane, sample -to-extraction solvent volume ratio; 2:1, extraction time; 20 min, desorption solvent; acetonitrile, desorption volume; 200 μL, and desorption time; 15 min) detection limits were 3.5 and 6.0 ng mL−1 for permethrin and cypermethrin, respectively. Relative standard deviations for intra- and inter-day reproducibility were below 8.3%. Device-to-device precision was in the range of 8.1–9.6%. The proposed microchip device was successfully applied to determine permethrin and cypermethrin in water samples with recoveries in the range of 73–96%. © 2021 Elsevier B.V.