高效液相色谱-荧光检测法同时测定蔬菜中3种磺胺类药物残留

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

建立了蔬菜中3种磺胺类药物(SAs)的高效液相色谱-荧光检测法。蔬菜样品用甲醇提取3次,将提取液浓缩干,用0.1mol/LHCl溶解残渣,经荧光胺衍生化后,用反相柱(ODS)分离,以乙腈和0.5%醋酸为流动相进行梯度洗脱,用荧光检测器检测。3种SAs的检出限(LOD)为1.02～1.29μg/g,方法的定量限(LOQ)为3.4～4.3ng/g(鲜重)。蔬菜样品中SAs的添加浓度在0.2～1.0ng/g范围内,3种SAs的平均回收率均大于87%,日内与日间RSD均小于10%。实际蔬菜样品测定结果表明,3种SAs在不同蔬菜中均有不同程度检出,总含量为0.0726～0.3709μg/g(鲜重)。

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. ） .