基于低毒溶剂的MSPD/HPLC法同时测定鱼肉中8种磺胺类药物残留

Simultaneous Determination of Eight Sulfonamide Residues in Fish Muscle Using Matrix Solid-phase Dispersion Coupled with High Performance Liquid Chromatography Based on Low Toxic Solvent

本实验以基质固相分散(MSPD)和高效液相色谱(HPLC)为基础,采用低毒的乙酸乙酯为洗脱溶剂,建立了与环境友好的鱼肉组织中8种磺胺类药物多残留快速分析法。将0.5g鱼肉与适量C18填料混合,研磨,制成半固态装柱,磺胺类药物经乙酸乙酯洗脱浓缩,用反相高效液相色谱测定。采用C18柱,柱温30℃;50mmol/L NaH2PO4-乙腈(70:30,V/V)为流动相,流速0.7ml/min;紫外检测(λ=270nm)。8种磺胺被有效分离,在0.010～1.000μg/ml范围内线性相关系数在0.9999以上;添加回收率为76.0%～115.0%,RSD<6.4%(n=6);仪器检测限均为0.010μg/ml;方法检测限为0.020μg/g。

A multi-residue analytical method for eight sulfonamides in fish muscle based on matrix solid-phase dispersion(MSPD) coupled with high performance liquid chromatography(HPLC) was developed.This method was environmentally friendly using ethyl acetate as the elution solvent.0.5 g of fish muscle mixed with 2 g of C18 packing material was grounded and filled into a SPE column.After washing with hexane,sulfonamides were eluted with ethyl acetate and determined using RP-HPLC with UV detector at 270 nm.Sulfonamide...