The synthesis of a molecularly imprinted polymer (MIP) composed of tetramethoxysilane (TMOS) and methyltrimethoxysilane (MTMOS) for recognized sulfonamides by sol-get process has been investigated. The MIP's preparation conditions, the H2O/Si molar ratios (R), pH value of competition solution, calcination temperature, and the TMOS and MTMOS molar fractions are discussed. Adsorption and selectivity in different pH solutions were determined by competition experiments between the MIP template (sulfamethazine, SMZ) and the analogue (sulfamethoxazole, SMO) using High-Performance Liquid Chromatography (HPLC). The results show that the selectivity of the MIP in competition solution with pH = 7.4 was higher than that with pH = 4.6. In addition, the second stage temperature of calcination. which was carried out at 375 degrees C, was obtained high selectivity. Moreover, the selectivity of the MIP (10.5) was approximately 3.5 times greater than the nonimprinted polymer (3.72) under the optimum preparation conditions.