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

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

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。

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 chromatogra- phy （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 800μg/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 2.5-20 μg/kg. The method exhibited good repeatability, high sensitivity, little interference and was widely suitable for the determination of sulfonamide residues in aquatic products.