高效液相色谱法测定蛋清和蛋黄中五种磺胺类药物残留

Determination of the residues in five sulfonamides in egg albumen and yolk by HPLC

建立了一种高效液相色谱法测定蛋清和蛋黄中5种磺胺类药物(磺胺嘧啶、磺胺二甲基嘧啶、磺胺甲氧达嗪、磺胺间甲氧嘧啶、磺胺甲恶唑)残留的分析方法。蛋清和蛋黄样品经乙腈提取后,上清液氮气吹干,用流动相溶解残渣,蛋黄用正己烷去脂净化后,用HPLC测定,蛋清提取液浓缩定容后,用HPLC测定。测定条件为,色谱柱:20RBAX SB-C185μm,250 mm×4.6 mm(i.d);流动相:甲醇/1%冰乙酸(蛋清:28/72,V/V;蛋黄:23/77,V/V);检测器:紫外检测器;检测波长270 nm。在0.02-5.0μg/ml范围内,标准曲线呈线性关系。在0.5,0.1,0.05 mg/kg 3个添加水平,该方法在蛋清中的回收率为84.3%-100.4%,变异系数为1.1%-7.0%;蛋黄中的回收率为80.0%-91.8%,变异系数为1.1%-11.5%;蛋清中的检测限为0.01 mg/kg,蛋黄中的检测限为0.03 mg/kg。

A high performance liquid chromatography method was developed for determination of sulfadiazine, sulfamethazine, sulfamethoxypyridazine, sulfamethoxazole, and sulfamonomethoxine in egg albumen and yolk. Samples were extracted with acetonitrile, the supernatant was evaporated to dryness and residues were dissolved in the mobile phase. Albumen extracts were directly analyzed by HPLC, while hexane was added to the yolk extracts to remove lipin, then the yolk extract was analyzed by HPLC. The HPLC system included a reversed phase column （ZORBAX SB-C18 50μm,250 mm× 4.6 mm（i. d） ）, a mobile phase of methanol and 1% acetic acid buffer, and a UV detector set at 270 nm. The recoveries of five sulfonamides at 0.5, 0.1, and 0.05 mg/kg levels were 84.3% - 100.4% and 80% - 91.8% in albumen and egg yolk, respectively, whereas the CV were 1.1% - 7.0%and 1.1% - 11.5%, respectively. The detection hmits for egg white and egg yolk were 0.01 mg/kg and 0.03 mg/kg, respectively.