Determination of chlorotoluron, isoproturon and metoxuron in soil by GLC-NPD and confirmation using GLC-MS

The analysis of several phenyl urea herbicides in soil by GLC-NPD, directly or after alkylation, and the confirmation of residues by GLC-ITD is reported. Soil was extracted with methanol, the organic solvent evaporated, the residue dissolved in hexane and then analyzed by gas chromatography on a 3% OV-17 glass packed column. An aliquot of the extract was ethylated overnight with EtI, NaH and Me2SO as solvent. The mixture was hydrolyzed, the ethylated compounds extracted with hexane and determinated by GLC-NPD on a BP-5 fused silica capillary column. Values obtained with the direct GLC analysis were reproducible and similar to those obtained after ethylation. Recovery of each herbicide was higher than 80% and the limit of detection was 0.01 ppm. These compounds were also analyzed by GLC-ITD. The sensitivity in the SIM mode was near 0.1 ng and the residues can be confirmed with this technique down to 0.01 ppm. © 1991 Springer-Verlag.