荧光胺衍生化液相色谱法检测动物肝脏中10种磺胺残留方法探讨

建立动物肝脏中常见的10种磺胺类药物(磺胺胍、磺胺嘧啶、磺胺二甲嘧啶、磺胺甲氧哒嗪、磺胺间甲氧嘧啶、磺胺-5-甲氧嘧啶、磺胺氯哒嗪、磺胺甲恶唑、磺胺二甲氧嘧啶、磺胺喹恶啉)残留量液相色谱同时测定方法。样品通过溶剂提取净化、荧光胺柱前衍生化,用配有荧光检测器的高效液相色谱仪测定,外标法定量。其线性范围分别为2～200μg/L、4～400μg/L、10～1000μg/L,线性相关系数r>0.999;方法检出限(LOD)为2～10μg/kg;其中9种磺胺,在5～100μg/kg的3个添加水平范围内的平均回收率为70.6%～90.2%;相对标准偏差为4.1%～7.6%。

Fluorescamine derivatization determination of 10 sulfonamide residues in animal liver by HPLC with fluorescence detector

A HPLC method has been established for determination of 10 sulfonamide drug residues in animal liver,including sulfaguanidine monohydrate,sulfadiazine,sulfadimidine,sulfamethoxypyridazine,sulfamonomethoxine,sulfamethoxydiazine,sulfachloropyridazine,sulfamethoxazole,sulfadimoxinum,sulfaquinoxaline.The sample was treated with solvent extraction and pre-column derivatization with fluorescamine,then detected by HPLC-fluorescence detector.The quantitative method was external standard method.The linear ranges of 10 sulfonamides are 2～200μg/L,4～400μg/L,10～1000μg/L,and the linear correlation coefficient r>0.999. The limits of detection(LOD) for the method are 2~10μg /kg.In the ranges of 5~100μg/kg for 9 sulfonamides,the average recoveries are 70.6%～90.2%,the relative standard deviations are 4.1%～7.6%.