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

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。

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

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. Sulfonamides were separated on C18 column using 50 mmol/L NaH2PO4-acetonitrile (70:30, V/V) as mobile phase at a flow rate of 0.7 ml/min, and the column temperature was 30 ℃. The linear range of this method is from 0.010 μg/ml to 1.000 μg/ml with the correlation coefficient of over 0.9999. The spike recoveries are in the range of 76.0% to 115.0% and the relative standard deviation (RSD) is less than 6.4% (n = 6). The limit of detection is 0.020 μg/g in a 0.5 g of sample.