Abstract

Objective: To validate in-house QuEChERS method, which scrutinizes and quantify the residue levels of some most frequently used organophosphorus pesticides and to prove a complete workflow for routine multi-residue pesticide analysis in representative bottle guard matrices and study the persistence of 23 organ phosphorus pesticides.Methods: QuEChERS (quick, easy, cheap, effective, rugged and safe) extraction method was followed. Method validation and residue screening of bottle guard samples were conducted by GC-FPD (Gas Chromatography-Flame Photometric Detector) were used to analyse the presence of pesticides whereas confirmation of pesticides was done by GC-MS (Gas Chromatographic-Mass Spectrometer). Results: For bottle guard matrix, LOD (limit of detection) and LOQ (limit of quantification) values are lowest for phorate (0.005 mg/kg and 0.015 mg/kg) and highest for parathion-methyl (0.1 mg/kg and 0.3 mg/kg) respectively. Calibration curve, was plotted between an area of 23 pesticide standard mixture against seven different concentration levels of 0.01, 0.02, 0.05, 0.10, 0.20, 0.50, 1.00 mg/kg with regression coefficient (R2) are in the range of 0.978-0.994. The mean recovered amount at 0.05 mg/kg spikeing concentration are in the range of lowest 0.0413 mg/kg to highest 0.0467 mg/kg and relative standard deviation are in the range of lowest 2.2 to highest 8.571.Conclusion: For ensuring exposure to contaminants, especially by dietary intake, Robust analytical methods were validated for carrying out both research and monitoring programmes and thus for defining limitations and supporting enforcement of regulations.

Highlights

  • The use of pesticides results in the ‘green revolution’ during the 1960s due to which crop losses reduces, yield improved but results in adverse effects on environmental quality and human health [1,2,3,4,5]

  • Method validation and residue screening of bottle guard samples were conducted by gas chromatography (GC)-FPD for the presence of pesticides whereas concentrated samples were analyzed by GC-mass spectrum (MS) in full scan mode for further confirmation of pesticides

  • 23 organ phosphorus pesticides which are commonly used in India viz anilophos, chlorfenvinfos, chlorpyrifos, chlorpyrifos-methyl, dichlorvos, ethion, malathion, parathion-methyl, monocrotophos, phorate, profenofos, quinolphos, trizophos, fenitrothion, phosalone, paraxon-methyl, fenamiphos, edfinphos, dimetoate, diazinon, fenthion, parathion and phosphomidon are considered for the study

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Summary

Introduction

The use of pesticides results in the ‘green revolution’ during the 1960s due to which crop losses reduces, yield improved but results in adverse effects on environmental quality and human health [1,2,3,4,5]. Tetraethyl pyrophosphate (TEPP) was the first OP insecticide, which was developed in Germany during World War Two as a by-product of nerve gas development [10]. By gas chromatography (GC) or high-performance liquid chromatography (HPLC) with selective detectors, the analyte determination is performed. International organizations: the European Union (EU) and the Codex Alimentarius Commission of the Food and Agriculture Organization (FAO) and the World Health Organization (WHO) controlled pesticide residues in food at permissible levels by the MRLs, which are established by them [12]. The pesticides studied were chosen based on their widespread use for crop protection [13]

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