A high performance liquid chromatography-inductively coupled plasma-mass spectrometric(HPLC-ICP-MS) method was established for the detection of two lead compounds,i.e.trimethyllead and triethyllead in blood and urine.The samples were extracted with benzene as solvent,followed by baci extraction with sodium thiosulfate after sonication and centrifugation.The extracts were separated by HPLC using an Agilent Zorbax Plus C18 column(4.6 mm×100 mm,3.5 μm),with 0.1 mol/L ammonium acetate-0.1 mol/L acetic acid and methanol as mobile phases by isocratic elution,and then detected by ICP-MSResults showed that there were good linear relationships for two lead compounds in blood and urine samples in the ranges of 3-200 ng/mL and 5-400 ng/mL,with their limits of detection and limits of quantitation of 0.85-1.31 ng/mL and 3.00-5.00 ng/mL,respectively.The recoveries ranged from 85.3% to 104% with intra-day and inter-day relative standard deviations(RSD) of 1.8%-10%,and the matrix effects of 88.3%-117%.The developed method was simple,sensitive and accurate,and it was suitable for the determination of trimethyllead and triethyllead in human blood and urine.