Hollow fiber-solid phase micro-extraction (HF-SPME) technique containing derived Fe3O4/ graphene nanocomposite as a novel high efficiency sorbent, coupled with gas chromatography was used to extraction and determination of three organophosphate pesticides; diazinon, fenitrothion and aqueous samples. First, magnetite nanoparticles (Fe3O4-NPs) were synthesized by chemicalco-precipitation of Fe(II) and Fe(III) ions (where the ratio of Fe(III) to Fe(II) is 2:1, surface of Fe3O4-NPs were modified with graphene (GO/MNPs). In this method, organophosphate pesticides were extracted by the synthesized nanocomposite and analytes by gas chromatography. Experimental parameters related to microextraction such as type of extraction time, organic solvent and agitation rate have been investigated and optimized. The extraction method has been validated for several types of real samples, and no matrix effect was observed. The technique requires minimal sample handling and solvent consumption. Using optimum conditions, low detection limits (0.00011–0.00016 μgL−1) and good linearity (R2 > 0.96) were obtained. Repeatability ranged from 3.11 to 4.91%. Finally the obtained results indicated that the method can be successfully applied for microextraction and determination of pesticides in environmental samples.
Keywords: HF-SPME, organophosphate pesticide, Fe3O4
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