Development and validation of a method for theudsimultaneous determination of 20 organophosphorusudpesticide residues in corn by accelerated solventudextraction and gas chromatography with nitrogenudphosphorus detectionud

摘要

The method for simultaneous determination of 20 organophosphorus pesticide residues in corn samples has been developed and validated. For the extraction of organophosporus pesticide residues from the samples, the accelerated solvent technique with the mixture of dichloromethane: acetone (1:1, V/V) was used. Clean up was done using liquid – liquid extraction with n – hexane, followed by solid phase extraction on primary secondary amine adsorbent, and elution with the mixture of acetone: toluene (65:35). The determination of the pesticides was carried out by gas chromatography with nitrogen phosphorus detection. Separation and quantitative determination of the analytes were performed on a fused silica capillary ZB-35 column (30 m x 0.25 mm i.d. x 0.25 μm, Phenomenex). The recovery was investigated in blank corn samples fortified with mevinphos, diazinon, dimethoate, bromofos-methyl, chlorfenvinphos, fenamiphos, ethion and phosalone at 5 ng/g, 10 ng/g, 15 ng/g , 20 ng/g and 25 ng/g, respectively and with methacrifos, phorate, etrimfos, parathion-methyl, pirimiphos - methyl, fenitrothion, chlorpyrifos, malathion, parathion, bromofos-ethyl, phosmet and azinphos-methyl at 10 ng/g, 20 ng/g, 30 ng/g, 40 ng/g and 50 ng/g, respectively. The recovery ranged from 76.0% to 112.0%. Repeatability expressed as relative standard deviation (RSD) was less than 8.2%. Linearity expressed as correlation coefficient (R2) ranged from 0.9935 to 0.9996. Measurement uncertainty (Ux) was lower than 14.2% for all tested pesticides. The limits of quantification (LOQ) were bellow 5 ng/g for all tested pesticides. The satisfactory Z-score results of international proficiency tests confirm good analytical performances of the developed method.udKeywords: Organophosporus Pesticide Residues, Gas Chromatography, Accelerated Solvent Extraction, Solid Phase Extractionud