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Determination of pyrimethanil and kresoxim-methyl in soils by headspace solid-phase microextraction and gas chromatography-mass spectrometry

Navalón, Alberto, Prieto, Avismelsi, Araujo, Lilia, Vílchez, José Luis
Analytical and bioanalytical chemistry 2004 v.379 no.7-8 pp. 1100-1105
detection limit, gas chromatography-mass spectrometry, headspace analysis, kresoxim-methyl, monitoring, polyacrylic acid, pyrimethanil, response surface methodology, soil, soil sampling, solid phase microextraction, statistical analysis
A method using headspace solid-phase microextraction (HS-SPME) then gas chromatography–mass spectrometry with selected ion monitoring (GC–MS, SIM) has been developed for determination of trace amounts of the fungicides pyrimethanil and kresoxim-methyl in soil and humic materials. Both fungicides were extracted on to a fused-silica fibre coated with 85 μm polyacrylate (PA). Response-surface methodology was used to optimise the experimental conditions. For soil samples the linear dynamic range of application was 0.004–1.000 μg g⁻¹ for pyrimethanil and 0.013–1.000 μg g⁻¹ for kresoxim-methyl. The detection limits were 0.001 μg g⁻¹ and 0.004 μg g⁻¹ for pyrimethanil and kresoxim-methyl, respectively. HP-SPME–GC–MS analysis was highly reproducible—relative standard deviations (RSD) were between 6.7 and 12.2%. The method was validated by analysis of spiked matrix samples and used to investigate the presence of pyrimethanil and kresoxim-methyl above the detection limits in soil and humic materials.