AbstractA simple robust 31P nuclear systems based NMR method is presented for the detection of alkyl methylphosphonic acids; metabolites of three organophosphorus nerve agents (GB or Sarin, GD or Soman, and GF or Cyclosarin) in the biological spiked samples of plasma and urine. The method gives linear response (correlation coefficients ~0.89) over the concentration range 10 g/ml to 300 g/ml in urine and plasma considering phosphorus nucleus. The quality control data demonstrated accurate identification of biomarkers of nerve agents at low concentration. NMR based method provides direct analysis of Biological samples without any sample pretreatment or sample preparation and sample tempering.