Abstract: A novel method for the determination of tetraethyl lead in water was developed by dispersive liquid-liquid micro-extraction（DLLME）coupled with gas chromatography-mass spectrometry (GC/MS). Some important parameters that effect the extraction efficiency，such as types and volumes of extraction， disperser solvent and extraction time were studied. Under the optimum conditions, the enrichment factors is 330. The method linearity ranges of tetraethyl lead are 0.40—40.0 μg/L with the detection limit(S/N=3) of 0.01 μg/L. The correlation coefficients are 0.999 3. The average recoveries of tetraethyl lead are range from 93.5% to 107% with the relative standard deviations of 3.2%—7.3%.