鱼肉中甲砜霉素残留的分析方法研究

利用固相萃取-气相色谱-质谱联机分析鱼肉中的甲砜霉素残留量。用乙酸乙酯振荡提取鱼肉中的甲砜霉素残留,用硅胶和C18固相萃取柱对乙酸乙酯提取物进行净化和富集。净化后的提取物衍生化和气相色谱-质谱选择离子定量检测(选择离子为409、411、499、501)。通过对提取净化富集条件的优化,建立了鱼肉中甲砜霉素的残留的检测方法。样品加标的回收率为80%～95%,相对标准偏差为3.6%～8.1%,最低检出限为0.3μg/kg。

Study on Analytical Method for Determination of Thiamphenicol Residues in Fish

Solid phase extraction(SPE)and gas chromatography mass spectrometric method were applied for the determinationof thiamphenicol residues in fish samples. The fish thiamphenicol was extracted by ethyl acetate under shaker .The ethyl acetateextracts were further purified and enriched by silica and C18 solid phase extraction cartridges. The final extracts were derivatisedand thiamphenicol was quantitatively determined by gas chromatography mass spectrometry in selected ion mode(ions selected409、411、499、501). The extraction and purification conditions were optimized. The recoveries of this method forfortified samples were between 80% ～ 95%, and the relative standard deviations were between 3.6%～8.1%.The detection limitof the method was below 0.3μg/kg.