高效液相色谱-在线柱后衍生荧光检测法同时测定水产品中14种磺胺类药物残留

建立水产品中14种磺胺类药物的高效液相色谱-柱后衍生荧光检测法。均质后的水产品试样用乙酸乙酯提取、盐酸溶液反萃取、正己烷脱脂、反相色谱柱分离、在线柱后衍生、荧光检测器检测、内标法定量。14种磺胺类药物(磺胺、磺胺嘧啶、磺胺噻唑、磺胺甲基嘧啶、磺胺5-甲氧嘧啶、磺胺二甲基嘧啶、磺胺甲氧哒嗪、磺胺氯哒嗪、磺胺6-甲氧嘧啶、磺胺甲基异噁唑、磺胺多辛、磺胺异噁唑、磺胺二甲氧哒嗪、磺胺喹噁啉)的线性范围为2.5～800μg/L,线性相关系数均大于0.9934;在2.5～200μg/kg三个添加水平范围内的平均回收率为88.9%～98.6%,相对标准偏差均小于6.96%。14种磺胺类药物的定量检出限为2.5～20μg/kg。方法重现性好、灵敏度高,杂质干扰少,广泛适用于水产品中磺胺类药物残留的检测。

Simultaneous Determination of 14 Sulfonamide Residues in Fishery Products by High Performance Liquid Chromatography with online Postcolumn Derivatization and Fluorescence Detection

A new method for the determination of 14 sulfonamide(sulfanilamide,sulfadiazine,sulfathiazole,sulfamerazine,sulfameter,sulfamethazine,sulfamethoxypyridazine,sulfachlorpyridazine,sulfamonomethoxine,sulfamethoxazole,sulfadoxine,sulfafurazole,sulfadimethoxine,and sulfaquinoxaline) residues in fishery products using high performance liquid chromatography(HPLC) equipped with fluorescence detector was established.Homogenized samples were extracted with ethylacetate,reverse-extracted into hydrochloric acid,defatted with hexane,separated by reversed-phase column chromatography,treated by on-line post-column derivatization,detected using a fluorescence detector,and quantified using the internal standard method.The linear range of the method for detecting the sulfonamides was from 2.5 to 800 μg/L,and the relative coefficients were all above 0.9934.The mean recoveries across spike levels varying from 2.5 to 200μg/kg were between 88.9% and 98.6% with RSDs less than 6.96%.The limits of quantification for the sulfonamides were 2.5-20μg/kg.The method exhibited good repeatability,high sensitivity,little interference and was widely suitable for the determination of sulfonamide residues in aquatic products.