固相萃取-高效液相色谱法测定动物肉组织中磺胺类药物的残留

Determination of Residual Sulfonamides in Meat by High Performance Liquid Chromatography with Solid-Phase Extraction

建立了一种快速、灵敏、环保的固相萃取-反相高效液相色谱同时分析动物肉组织中5种磺胺类药物残留的方法.将样品加入到盛有无水硫酸钠的离心管中,再用乙酸乙酯提取;提取液经氨基固相萃取柱净化后,用1.5%(体积分数)乙酸乙醇溶液洗脱.洗脱液用高效液相色谱分离,二极管阵列检测器检测,外标法定量.5种磺胺类药物的线性关系良好,磺胺二甲基嘧啶(SM2)、磺胺间甲氧嘧啶(SMM)、磺胺甲(口恶)唑(SMZ)的线性范围均为30～5 000 μg/L,磺胺二甲氧嘧啶(SDM)、磺胺喹(口恶)啉(SQ)的线性范围均为60～5 000 μg/L.2种动物肉组织(鸡肉、猪肉)中5种磺胺类药物的加标回收率在73.2%至97.3%范围内,当添加水平为50 μg/kg时,加标回收率的相对标准偏差在2.5%至11.6%范围内;SM2,SMM和SMZ的检测限(S/N=3)和定量限(S/N=10)分别为3 μg/kg和10 μg/kg,SDM和SQ的检测限和定量限分别为7 μg/kg和25 μg/kg.

A method was developed for determining residual sulfonamides （SAs） such as sulfa-methazine （SM2）, sulfamonomethoxine （SMM）, sulfamethiazole （SMZ）, sulfadimethoxine （SDM） and sulfaquinoxaline （SQ） in pork and chicken using solid-phase extraction （SPE） and high performance liquid chromatography （HPLC） with a photodiode array detector. The samples were extracted with ethyl acetate. An NH2 column was used for clean up. For the HPLC determination, an Intersil ODS-2 column was used with a mixture of methanol-acetonitrile-water-acetic acid （2： 2： 9： 0.2, v/v） as the mobile phase. The detection limits （S/N=3） were 3μg/kg for SM2, SMM and SMZ, and 7μg/kg for SDM and SQ. The quantitation limits （S/N=10） were 10μg/kg for SM2 , SMM and SMZ, and 25μg/kg for SDM and SQ. The linear ranges were 30-5000μg/L for SM2, SMM and SMZ, and 60-5000μg/L for SDM and SQ. The recoveries were between 73.2% and 97.3% with the relative standard deviations between 2.5% and 11.5% originated from the spiked level of 50μg/kg.