Abstract:A method of simultaneous determination of 15 sulfonamides residues in aquatic products was established by solid phase extraction-high performance liquid chromatography (SPE-HPLC). The samples were extracted with ethyl acetate, degreased with n-hexane, and purified by polymer cation exchange (PCX) solid phase extraction column. The analysis was performed by high performance liquid chromatography with a chromatographic condition of separation on a Waters C18 column (4.6 mm×250 mm, 5.0 μm) under gradient elution mode with methanol and PBS solution containing 1.1% acetic acid (0.01 mol/L) as the mobile phase. The target analytes were detected at the wavelength of 270 nm. The 15 sulfonamides were completely separated within 65 min, showing a good linear relationship within 0.5~10.0 μg/mL with correlation coefficients greater than 0.990 0. The limits of detection were in the range of 10~20 μg/kg, and the limits of quantitation were 20~60 μg/kg. The blank recovery rates of spiked samples at three mass fraction levels (500, 1 000, 2 000 μg/kg) ranged from 73.1% to 109.6% with the relative standard deviations (RSDs) of 1.0%~6.7%. The established detection method in this study showed good reproducibility, stability, and low detection limit. The residues of SAs in 10 different species of aquatic products from Jiangxi province were sampled and detected, and no residues were detected, indicating that the residues of SAs in aquatic products from Jiangxi province were not severe.
