柱后衍生法检测鳗鱼肌肉中磺胺类药物残留量研究

建立了鳗鱼肌肉中磺胺类药物残留的高效液相色谱柱后衍生分析方法。鳗鱼肌肉样品经乙腈和水提取，液- 液分配和固相萃取净化浓缩后，采用高效液相色谱柱后衍生法检测磺胺类药物经C18 色谱柱分离，在柱后反应单元中与荧光胺反应，生成具有荧光特性的分子，荧光检测器检测方法定量检测限为2.0μg/kg，磺胺浓度在0.005～0.2μg/ml 范围内线性关系良好(r ≥ 0.9998)，磺胺浓度范围在2.0～50.0μg/kg 鳗鱼肌肉加标样，日内和日间回收率为85.1%～90.2%，相对标准偏差2.74%～6.04%。实验结果表明，该检测方法适用于低浓度水平鳗鱼肌肉中磺胺类药物残留检测。

High Performance Liquid Chromatography Coupled with Post-Column Derivation for Determination of Sulfonamides Residues in Eel Muscle

A method was established to determine sulfonamides in eel muscle by post-column derivatization high performance liquid chromatography. The sulfonamides residues in eel were extracted with acetonitrile and water, isolated by liquid-liquid partition and solid-phase extraction, then determined by post-column derivatization high performance liquid chromatography. The sulfonamides were separated by C18 column, converted to fluorescent derivatives by post-column derivatization with fluorescamine, detected by fluorescence detector. The limits of quantification is 2.0 μg/kg. The correlation coefficients of linear calibration curves are over 0.9998 within the concentration range of 0.005 to 0.2 μg/ml. For the 2.0 to 50.0 μg/kg spiked eel sample, both within-day and day-to-day recoveries are from 85.1% to 90.2%, and RSDs are from 2.74% to 6.04%. The experimental results presented above indicate that this method can be used to detect the low concentration sulfomamides in eel muscle.