基质固相分散-高效液相色谱法测定鱼肉组织中磺胺类药物的残留

Matrix solid-phase dispersion and high performance liquid chromatographic determination of sulfonamide residues in fish muscles

建立了一种同时测定鱼肉中磺胺嘧啶、磺胺甲基嘧啶、磺胺二甲嘧啶、磺胺甲基异噁唑、磺胺喹噁啉5种磺胺类药物残留的高效液相色谱测定方法。样品经二氯甲烷提取,C18填料固相分散萃取净化后,浓缩定容。经乙腈、3%乙酸缓冲溶液(v/v)梯度洗脱分离,紫外检测器检测,外标法定量。结果表明,5种磺胺类药物在0.10～5.0μg/mL范围内线性关系良好,添加回收率为75%～93%。方法检测限:磺胺嘧啶、磺胺甲基嘧啶、磺胺二甲嘧啶为0.020mg/kg,磺胺甲基异噁唑、磺胺喹噁啉为0.025mg/kg。

A high performance liquid chromatographic method has been developed for the simultaneous determination of five sulfonamides residues in fish muscles, including sulfadiazine, sulfamerazine, sulfmethazine, sulfamethoxazole and sulfaquinoxaline. The samples were extracted by dichloromethane then cleaned up by C18 solid phase exaction. Gradient elution with a mobile phase of 3% acetic acid buffer-acetonitrile（v/v） was employed. The residues were determined by high performance liquid chromatography with ultraviolet detection and quantified by external standard method. The linear ranges were 0.10-5.0 μg/mL. The average recoveries in spiked samples were 75%-93%. The detection limits were 0.020 mg/kg for sulfadiazine, sulfamerazine and sulmethazine, and 0.025 mg/kg for sulfamethoxazole and suifaquinoxaline.