In this study, magnetic-dispersive solid-phase extraction coupled with ion pair-dispersive liquid–liquid micro-extraction (MSPE-i-DLLME) was used to the pre-concentration and extraction of five sulfonamides residues (sulfadiazine, sulfathiazole, sulfacetamide, sulfamethazine and sulfamethoxazole) in animal foodstuffs. The sulfonamides are extracted using magnetic carbon nanocomposite and then eluted with acetonitrile. In the DLLME step, the target analytes are collected in 1-octanol containing 10% Aliquat-336 (as extraction solvent). Finally, the compounds are quantified by HPLC with DAD detection. The extraction parameters optimized using the one at the time and central composite design methods. Under the optimized conditions: sample solution volume was 100 mL; initial pH: 12, amounts of MCNs: 30 mg; desorption solvent (ACN) volume, 1 mL; desorption condition, 10 min sonication at two step; extraction solvent (1-octanol + 10% aliquat) volume, 115 µL; pH of DLLME step, 3; salt effect, 24.6%, (w/v) NaCl; centrifuge, 5 min, 4000 rpm. In these extraction conditions, the proposed procedure represented good pre-concentration factors between 130 and 490; detection limits in the range from 0.01 to 5 μg kg⁻¹ (at S/N = 3), and linear response in the 0.1–400 μg kg⁻¹ concentration range. The method is successfully applied to the determination of sulfonamides residues in animal foodstuffs.

在这项研究中，将磁分散固相萃取与离子对分散液-液微萃取（MSPE-i-DLLME）结合使用来对5种磺酰胺残留物（磺胺嘧啶，磺胺噻唑，磺乙酰胺，动物食品中的磺胺二甲嘧啶和磺胺甲恶唑）。使用磁性碳纳米复合材料萃取磺酰胺，然后用乙腈洗脱。在DLLME步骤中，将目标分析物收集在含有10％Aliquat-336（作为萃取溶剂）的1-辛醇中。最后，通过DAD检测的HPLC对化合物进行定量。使用当时的最佳提取参数和中央复合设计方法。在最佳条件下：样品溶液体积为100 mL；初始pH：12，MCN含量：30 mg；解吸溶剂（ACN）体积，1 mL；解吸条件，两步超声处理10分钟；萃取溶剂（1-辛醇+ 10％aliquat）体积为115 µL；DLLME步骤的pH为3; 盐效应，24.6％，（w / v）NaCl; 离心机，5分钟，4000 rpm 在这些萃取条件下，拟议的程序代表了130至490之间的良好预富集因子。检出限为0.01至5μgkg^-1（在S / N  = 3时），线性响应在0.1–400μgkg ^-1浓度范围内。该方法已成功应用于动物食品中磺胺类药物残留的测定。