A method has been developed for the rapid quantitative analysis of organophosphorous and carbamate pesticides using HPLC. Good separation was obtained among the four major groups of organophosphorus pesticides [i.e. aryl phosphorothionate (methyl parathion), alkyl phosphorothionate (malathion), enolphosphate (phosphomidon, monocrotophos, dichlorvos), heterocyclic phosphorothionates (quinalphos)] and carbamates [viz. Carbaryl (Sevin) and Baygon (Dalf)] with a detection limit of 100 ng for all the pesticides. Separation was measured in terms of capacity factor (k') resolution (R) and selectivity factor (alpha ii). The method described can be used for the analysis of biological samples for the presence of organophosphorus and carbamate pesticides in the cases of poisoning. Recovery studies were made in the blood, lung and liver and found to be 85-97% with reproducibility at greater than 95%.