鸡肉中多种磺胺兽药残留量测定的高效液相色谱-电化学检测法

Determination of Residues of Sulfonamides in Chicken by HPLC with Electrochemical Amperometric Detection

采用液相色谱电化学法测定了鸡肉中磺胺类药物残留量 ;磺胺用氯仿提取后 ,取部分提取液用氮气吹干 ,残渣溶于KH2PO4 中 ,用正己烷脱脂 ,水相进样 ,液相色谱分析用C18 柱 ,流动相为甲醇 -0.01mol/LKH2PO4 (pH6,体积比25∶75) ,检测电位1.0V ;与紫外检测器相比 ,电化学检测器(ECD)有更高的灵敏度和选择性 ,ECD的检出限为磺胺嘧啶0.02ng ,磺胺甲氧哒嗪0.06ng ,磺胺甲基异唑0.07ng。

A HPLC method with electrochemical detection(ECD) was proposed for the quantitative determination of residues of sulfonamide drugs in chicken. Sulfonamides in chicken sample were extracted with chloroform. The extract was filtered, and then evaporated to dryness under a stream of nitrogen. The residue was dissolved into KH2PO4 solution and defatted with hexane. The aqueous sample was taken for analysis by HPLC with ECD at potential of 1.0 V after filtration. LC analysis was performed on a C18 column using a mobile phase of methanol-10 mmol/L phosphate buffer(25∶75 by volume)at pH 6. Compared with ultraviolet detector ECD has a higher sensitivity and selective for sulfonamides. The detection limits of 0.02 ng, 0.06 ng and 0.07 ng were obtained for sulfadiazine, sulfamethoxypyridazine and sulfamethoxazole, respectively.