This study was carried out to explore the most sensitive and useful method for simultaneous determination of five sulfa drugs(sulfamethazine, sulfamerazine, sulfamonomethoxine, sulfadimethoxine, sulfaquinoxaline) in livestock productions(pork muscle, bovine muscle, chicken muscle, milk ) by HPLC with UV detector and reverse phase column. The results obtained were as follows：1. For mobile phase acetonitrile-0.01M ammonium acetate (23：77) showed more applicable sensitivity and retention times than acetonitrile-1% acetic acid(23：77). Thus acetonitrile-0.01M ammonium acetate(23：77) selected and applied to the modification test, from which it was found pH 6.75 was the most adequate. 2. Optimal wavelength of UV for SMT(sulfamethazine), SMR(sulfamerazine), SMM(sulfamonomethoxine), SD(sulfadimethoxine), and SQ(sulfaquinoxaline) were 266, 266, 265, 269 and 250nm, respectively, and that for simultaneous application it was 263nm. 3. The average recovery rate by extractant(chloroform, dichloromethane, chlorform+dich-loromethane) in the classic method was not significantly different(p>0.05) but that by chloroform higher than the others. Thus chloroform was found to be adequate as extractant in this classic method. 4. The average recovery rate was 86.5% by the MSPD(matrix solid phase disperse) method, which was significantly higher than that by the classic method(p<0.05). Also the recovery rates by method were significantly different(p<0.05) in accordance with sample and type of drug. The MSPD method was much superior to classic method on clean-up.