Development of fast, efficient and ecological method employing vortex-assisted dispersive liquid-liquid microextraction combined with fast gas chromatography-mass spectrometry for pesticide residues analysis in alcohol-content samples.

A fast, ecological, and efficient method employing vortex-assisted dispersive liquid-liquid microextraction (DLLME) method for isolation and preconcentration of selected endocrine disrupting pesticides from beverages containing some degree of alcohol was developed. The effect of several extraction parameters, such as selection of extractive solvent, its volume and extraction time, the salt addition was investigated. Four different extractive solvents (chloroform, tetrachloroethane, tetrachloromethane and toluene) and their combinations were evaluated for DLLME. Under the following conditions: 1mL of fortified sample, 80μL of tetrachloroethane, 1.5mL of water, vortex assistance for 3min at the speed of 1800rpm, and no salt addition, the method was validated. Linearity was studied in the concentration range of 0.01-250μg/L with coefficient of correlation ranging between 0.9940 and 1.0000, limits of detection and quantification ranging between 0.02-1.4μg/L and 0.07-4.7μg/L, respectively. Recoveries were satisfactory in the range of 70-120%, with the exception of diphenyl, alachlor and fenarimol at the lowest concentration level and p,p-DDE at concentration level of 100 and 250μg/L. The applicability of the developed and validated method was proved by the analysis of real samples.