An intercomparison study on the determinations of glyphosate, chlormequat and mepiquat residues in wheat
Résumé
An intercomparison study on the analytical determinations of glyphosate, chlormequat and mepiquat residues in cereals was performed. Four samples were sent to six participating laboratories, one blank, two incurred and one spiked sample. For glyphosate, two laboratories reported considerably lower results than the other four. One of the two laboratories with low results also reported low recoveries. The results of a sample spiked with 0.80 mg/kg glyphosate and an incurred sample, ranged from 0.23-0.87 mg/kg and 0.11-0.25 mg/kg respectively. The strong correlation between the two samples (r2=0.95) indicates a systematic between-laboratory variation. Several different principles were used for the analysis of glyphosate using different clean-up techniques and gas chromatography-mass spectrometry, high performance liquid chromatography-fluorescence or liquid chromatography-mass spectrometry for detection. The results of the chlormequat residues showed more consistency. All but one laboratory obtained comparable results. However the correlation between the results for the sample spiked with 0.38 mg/kg (range:0.26-0.65 mg/kg) and the incurred samples (range: 0.19-0.45 and 0.15-0.23 mg/kg, respectively) again showed a strong correlation (r2=0.99 and 0.88) indicating a systematic component. For mepiquat, results above the limit of quantification were only reported for the spiked sample. The results ranged from 0.29-0.92 mg/kg (spiked concentration=0.38 mg/kg). Three laboratories had results that deviated less than 25% from the fortified concentration. Two laboratories reported results 38% and 141% above the fortified concentration, respectively.
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