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Analysis of cypermethrin residues and its main degradation products in soil and formulation samples by gas chromatography-electron impact-mass spectrometry in the selective ion monitoring mode

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A fast, simple and inexpensive sample preparation method based on the matrix solid-phase extraction (SPE) technique is proposed for the isolation of cypermethrin and its metabolite residues from soils. Both the extraction and clean-up procedures were carried out in two steps and target compounds were determined by gas chromatography coupled with electron-impact mass spectrometry (GC-EI/MS). The characteristic ions and fragmentation mechanism of cypermethrin were evaluated by electron impact ionization mass spectrometry (EI/MS). After the optimization of different parameters, such as the extraction solvent, the pesticide was extracted from the matrix with methanol/acetone in a Soxhlet extractor, cleaned up on a Florisil column by elution with a mixture of 30% ethyl acetate in n-hexane and analyzed by gas chromatography-electron impact ionization mass spectrometry (GC-EI/MS) in the selected ion-monitoring mode (SIM) with permethrin as internal standard. Recovery was in the range 77–118% with relative standard deviations (RSD) between 2.5% and 10.2%. The limit of detection (LOD) was 6.5 µg/kg for cypermethrin. The developed method was linear in the injection range 6–30 ng, with correlation coefficients greater than 0.9957.
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Keywords: cypermethrin; formulations; gas chromatography-mass spectrometry; pesticide residues; soils; solid-phase extraction

Document Type: Research Article

Affiliations: 1: Department of Chemistry, Faculty of Sciences,University Mohamed Premier, Oujda,BP 717- 60000-Morocco, 2: Department of Analytical Chemistry and Food Technology, Faculty of Chemistry,Campus Universitario, University of Castilla-La Mancha, E-13004 Ciudad Real, Spain

Publication date: October 15, 2012

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