Abstract: The author established a solid phase extraction - high performance liquid chromatography（SPE- HPLC）method to determinate concentrations of ofloxacin，tetracycline，sulfamethoxazole in water. The samples were enriched with solid phase extraction column，after being eluted with ultrapure water - acetonitrile（75∶25，volume ratio），the samples were determinated with high performance liquid chromatography - ultraviolet detector. In the conditions of detection wavelength λ = 274 nm，column temperature 30 ℃，mobile phase as acetonitrile - phosphoric acid aqueous solution（50∶50，volume ratio），the author used a gradient elution program to achieve the baseline separation of three kinds tested components. Linear range of ofloxacin was 0. 25～2 μg/mL，tetracycline was 0. 4～ 2 μg/mL，sulfamethoxazole was 0. 04～2 μg/mL. Blank spiked recoveries were 82. 32% ～94. 86% .Detection limits of ofloxacin，tetracycline，sulfamethoxazole were 0. 04，0. 25，0. 01 μg/mL respectively， quantitation limits were 0. 25，0. 40，0. 04 μg/mL，respectively. This method is simple，rapid，sensitive and efficient to meet the needs of practical work.

Key words: solid phase extraction（SPE）, high performance liguid chromatography（HPLC）, tetracycline, ofloxacin；sulfamethoxazole