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Vortex-assisted low density solvent liquid-liquid microextraction and salt-induced demulsification coupled to high performance liquid chromatography for the determination of five organophosphorus pesticide residues in fruits.

Talanta (2014-12-06)
Ketsarin Seebunrueng, Yanawath Santaladchaiyakit, Supalax Srijaranai
ABSTRACT

A simple and rapid microextraction method, vortex-assisted low density solvent liquid-liquid microextraction and salt-induced demulsification (VLLME-SID) coupled to high performance liquid chromatography (HPLC) was developed for the determination of organophosphorus pesticide (OPP) residues in fruits. The studied OPPs were azinphos-methyl, parathion-methyl, fenitrothion, diazinon and chlorpyrifos. For VLLME-SID, a mixture of low density solvents (1-dodecanol and hexane) was used as the extraction solvent under vortex agitation for enhancing dispersion. After complete dispersion, the emulsion was formed and the OPPs were extracted into extraction solvent droplets. Then, the emulsion was quickly broken up into two clear phases after the addition of AlCl3 as a demulsifier. Centrifugation was not required in this procedure. Under the optimal conditions, high enrichment factors (180-282), low limit of detections (LODs) (0.05-1 ng mL(-1)) and good precision (RSD≤7% for retention time and peak area) were obtained. The proposed method was successfully applied to the analysis of OPP residues in fruit samples (watermelon, grape, and cantaloupe). The LODs for samples were in the range 0.0006-0.0015 mg kg(-1) which are below the established EU-MRLs (0.01-0.3 mg kg(-1)). Good recoveries were also obtained (80-104%).

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