An immunoaffinity column (IAC), which can bind diazinon primely, was developed to treat the water and soil samples. The IAC, having an appropriate binding capacity for diazinon (200 ng per mg gel), was prepared by entrapping the anti-diazinon antibody into sol-gel, which was made from hydrolyzed Tetramethoxysilane (TMOS). In comparison with the IACs entrapped with others non-special antibodies, the IAC entrapped with anti-diazinon antibody has a special binding capacity to diazinon. Two different elution modes, 40% and 20% MeCN water solution, were evaluated for desorbing diazinon from the IAC. Efficient desorption of bound diazinon was achieved with the 40% MeCN water elution. The water and soil samples spiked with diazinon were treated by the IAC. The reliable recoveries, which ranged from 50% and 100% with RSD from 4.54% to 16.79%, were achieved.