Abstract: A gas chromatography(GC) with electronic capture detection(ECD) for determination of chloramphenicol(CAP) residues in shrimps samples has been validated. The samples were extracted with ethyl acetate, defatted with hexane and passed through silica SPE column. The eluted solutions were derivatized with BSTFA+1%TMCS (99:1). The solution was determined with GC-ECD, using external standard calibration. When the added level of the standard were between 0.2×10^-9～1.0×10^-9, the recoveries were 50%～110%, the RSD were 0.9%～5.0%, the correlation coefficient r0.998.