Ultrasound-Assisted Emulsification-Microextraction/Ion Mobility Spectrometry Combination: Application for Analysis of Organophosphorus Pesticide Residues in Rice Samples

The present paper describes the validation of ultrasound-assisted emulsification-microextraction method followed by ion mobility spectrometry (IMS) detection for simultaneous determination of two organophosphorus pesticides, diazinon and chlorpyrifos. Ultrasound radiation was applied for accelerating the emulsification of microliter organic solvent in aqueous solutions and enhancing the microextraction efficiency. This preconcentration step combined with IMS detection provided a precise and accurate method for determination of trace amounts of diazinon and chlorpyrifos pesticides. The effect of parameters influencing the extraction efficiency such as sonication time, type of extraction solvent, extraction solvent volume, and salt concentration were investigated and discussed. The enrichment factors found, under optimum conditions, were 230 and 300 for diazinon and chlorpyrifos, respectively, with corresponding LOD of 2.1 and 3.2 μg L−1. The presented method can be applied for the determination of diazinon and chlorpyrifos in the range 6.0–700 and 8.9–750 μg L−1, respectively, with correlation coefficients (R2) > 0.99. The applicability of the proposed method was evaluated by determination of the residues of the investigated pesticides in rice paddy water gathered from four stations during 60 days after spraying (June 2014), and in storage rice samples in Mazandaran province, Iran.