Simultaneous Determination of Three Sulfonamides Residues in Vegetable by High Performance Liquid Chromatographic Method with Fluorimetric Detection / 分析化学

ABSTRACT

A high performance liquid chromatographic method with fluorimetric detector was developed for the simultaneous determination of three sulfonamides in vegetable samples. Vegetable samples were extracted with methanol for three times, and then the combined extracts were evaporated to dryness under reduced pressure at 45 ℃. The residue was dissolved in 0.1 mol/L HCl and the analytes were derivatized with fluorescamine. The chromatographic separation was performed on an ODS column with a gradient elution program using mobile phases based on mixtures of acetonitrile and 0.5% acetic acid aqueous solution. The derivatized compounds were detected with fluorimetric detector. The limit of detection was 1.02-1.29 μg/L and the limit of quantification was 3.4-4.3 μg/kg(fresh weight, F.W.) for three sulfonamides in vegetable. The average recoveries were higher than 87%, inter and intra RSDs were lower than 10% for all samples spiked with 0.2-1.0 μg/g of sulfonamides. The proposed method has been applied to the analysis of vegetables sold in Hefei markets. The result indicated that 3 SAs were found at different degree in the practical vegetable samples with the total concentrations between 0.0726-0.3709 μg/g(F.W.).