AbstractThe organophosphate insecticides dichlorvos, trichlorphon and isofenphos have been extracted from soil and ryegrass by blending with acetone+ benzene (19+1, v/v) and charcoal. After filtering, water and waxes were precipitated from the extract at − 78°. The extracts were analysed for insecticide by gas chromatography using alkali flameionisation detection. Trichlorphon was converted to the acetate by on‐column acetylation. Recoveries ranged from 73 to 93% for levels of insecticide from 0.1 to 10mg/kg. The carbamate insecticides methomyl and carbofuran plus the metabolite 2,3‐dihydro‐3‐hydroxy‐2,2‐dimethylbenzofuran‐7‐yl methylcarbamate have been extracted from soil and ryegrass samples by shaking with acidified ammonium acetate. Following filtration and neutralisation, the aqueous phase was extracted with dichloromethane. The carbamates in the extracts were determined by gas chromatography using on‐column trans‐esterification to methyl methylcarbamate. Recoveries ranged from 79 to 97% for levels of insecticid