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

作者：Garoiaz Hasnae; Berrabah Mohammed; Elidrissi Abderahmane; Hammouti Belkheir; Rios Angel^*

来源：International Journal of Environmental Analytical Chemistry, 2012, 92(12): 1378-1388.

DOI：10.1080/03067319.2011.581365

• pesticide residues
• soils
• formulations
• cypermethrin
• solid-phase extraction
• gas chromatography-mass spectrometry

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 mu g/kg for cypermethrin. The developed method was linear in the injection range 6-30 ng, with correlation coefficients greater than 0.9957.

• 出版日期2012