Dispersive micro solid-phase extraction procedure using a novel and selective sorbent prepared from four components was developed as a sample preparation strategy for extracting five organophosphorus pesticides, including fenitrothion, malathion, ethion, and chlorpyrifos, and diazinon in several vegetables, fruit juices, and cow's milk samples. Due to the high importance of the sorbent in the microextraction process, the percentages of sorbent components, including metal-organic framework (ZIF-67), chitosan, magnetic Fe3O4 nanoparticles, and silica nanoparticles, were optimized by a simplex lattice mixture design. After optimizing the sorbent composite, effective parameters on the extraction of organophosphorus pesticides were optimized using a definitive screening design and Box-Behnken design, respectively. A surfactant (Triton X100) as a dispersion agent with a low volume (10 μL) was utilized in the microextraction procedure to reduce the sorbent dispersion time and increase the sorbent dispersion efficiency. Under the optimal conditions, linearity for the determination of fenitrothion, malathion, ethion, chlorpyrifos, and diazinon was in the concentration ranges of 0.13-1100, 0.27-1000, 0.38-1000, 0.21-1200, and 0.11-1100 ng mL-1 with a determination coefficient higher than 0.9906, respectively. The quantitation limits, detection limits, and relative standard deviations (n = 5) were lower than 0.38 ng mL-1, 0.11 ng mL-1, and 4.59% for the determination of organophosphorus pesticides. The method application for measuring OPPs on cucumber, carrot, tomato, apple juice, orange juice, and cow's milk indicated the presence of residual amounts of malathion in a cucumber sample, diazinon in a carrot sample, and chlorpyrifos in a tomato sample.
Keywords: Definitive screening design; Dispersive micro solid-phase extraction; Food samples; Metal-organic frameworks; Organophosphorus pesticides; Simplex lattice mixture design.
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