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Development and Validation of a Method for the Simultaneous Determination of 20 Organophosphorus Pesticide Residues in Corn by Accelerated Solvent Extraction and Gas Chromatography with Nitrogen Phosphorus Detection
American Journal of Applied Chemistry
Volume 2, Issue 4, August 2014, Pages: 46-54
Received: Jul. 17, 2014; Accepted: Aug. 5, 2014; Published: Aug. 10, 2014
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Vesna Kostik, Medical Faculty, Department of Pharmacy, University “Goce Delchev”, Shtip, Republic of Macedonia
Biljana Gjorgeska, Medical Faculty, Department of Pharmacy, University “Goce Delchev”, Shtip, Republic of Macedonia
Bistra Angelovska, Medical Faculty, Department of Pharmacy, University “Goce Delchev”, Shtip, Republic of Macedonia
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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.
Organophosporus Pesticide Residues, Gas Chromatography, Accelerated Solvent Extraction, Solid Phase Extraction
To cite this article
Vesna Kostik, Biljana Gjorgeska, Bistra Angelovska, Development and Validation of a Method for the Simultaneous Determination of 20 Organophosphorus Pesticide Residues in Corn by Accelerated Solvent Extraction and Gas Chromatography with Nitrogen Phosphorus Detection, American Journal of Applied Chemistry. Vol. 2, No. 4, 2014, pp. 46-54. doi: 10.11648/j.ajac.20140204.11
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