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This study describes the development of a sensitive and accurate dispersive liquid-liquid microextraction strategy for the preconcentration and determination of selected pesticides in wastewater and lake water samples by gas chromatography-mass spectrometry. Determination of these pesticides at high accuracy and precision is important because they can be still be found in environmental samples. The type of extraction solvent and type of disperser solvent were optimized using the univariate approach. Furthermore, a Box-Behnken experimental design was used to set up a working model made up of 18 combinations of three variables, tested at three levels. The parameters fitted into the design model were volume of extraction solvent, disperser solvent volume, and mixing period. Analysis of variance was used to evaluate the experimental data to determine the significance of extraction variables and their interactions, before selecting optimum extraction conditions. The method was then applied to aqueous standard solutions between 2.0 and 500 μg L -1 , and the limit of detection (LOD) and quantification (LOQ) values obtained for the analytes were between 0.37-2.8 and 1.2-9.4 μg L -1 , respectively. The percent recoveries were calculated in the range of 92-114 and 96-110% for wastewater and lake water, respectively. These results validated the accuracy and applicability of the method to the selected matrices.

A simple and accurate method for the determination of bismerthiazol and its metabolite 2-amino-5-mercapto-1,3,4-thiadiazole was developed in Chinese cabbage and soil by high-performance liquid chromatography-diode array detection in this study. The limits of detection were 0.06 mg/kg for bismerthiazol and 0.03 mg/kg for 2-amino-5-mercapto-1,3,4-thiadiazole, respectively. Recoveries of cabbage and soil were investigated at three spiking levels and were in the range of 84.0-96.0% for bismerthiazol and 71.0-74.6% for 2-amino-5-mercapto-1,3,4-thiadiazole, with relative standard deviations below 7.0%. For field experiments, the half-life of bismerthiazol was 2.4-2.5 days in Chinese cabbage and 2.5-4.8 days in soil at the two experimental locations in China. Dissipation residues of 2-amino-5-mercapto-1,3,4-thiadiazole were lower than 0.72 mg/kg. Terminal residues of bismerthiazol and its metabolite were less than 3.0 and 0.3 mg/kg in Chinese cabbage, respectively. No bismerthiazol or metabolite residues were detected in soil on days 5, 7, 10, and 14 after the last spraying at the two dosage levels.