鸡蛋中磺胺二甲基嘧啶残留快速分析方法

    Rapid Detection Method for Sulfamethazine Residue in Eggs

    • 摘要: 【目的】探讨鸡蛋蛋液、蛋清和蛋黄中兽药残留的快速分析方法。【方法】以磺胺二甲基嘧啶为例,建立蛋液、蛋黄和蛋清样品中磺胺二甲基嘧啶的快速检测方法。样品的前处理采用液 - 液萃取技术快速实现目标化合物的提取与净化,目标化合物采用选择性好和灵敏度高的高效液相色谱 - 电喷雾 - 串联质谱进行检测。【结果】经基质加标实验验证,该方法稳定可靠。蛋液、蛋黄和蛋清中目标化合物的添加回收率分别为78.4%~85.2%、77.9%~89.0%、83.0%~88.1%,方法检测限均为 0.5 ng/g。采用该方法对广州市 15 例鸡蛋样品进行分析,结果显示,仅 1 例鸡蛋样品中检测到磺胺二甲基嘧啶,在蛋液、蛋黄和蛋清的含量分别为 0.66、0.94、0.47 ng/g。【结论】该方法的样品前处理不需要过柱,操作简洁、耗材低廉、方法灵敏度高,且该方法具有良好的加标回收率和较好重复性,适合大批量蛋液、蛋黄与蛋清样品中磺胺二甲基嘧啶的快速检测。

       

      Abstract: 【Objective】 The study was to develope a rapid detection method for veterinary drug residues in whole egg, albumen, and yolk. 【Method】 Taking sulfamethazine as a case, a method was developed for rapid detection of sulfamethazine in whole eggs, yolks, and albumens. The sample pretreatment was conducted by using liquid-liquid extraction to achieve the extraction and purification of target compounds. And the target compounds were detected by high performance liquid chromatography-electrospray ionization tandem mass spectrometry that with good selectivity and high sensitivity. 【Result】 As verified by spike matrix test, the method was proved to be stable and reliable. The recoveries of sulfamethazine in whole eggs, yolks, and albumens were in range of 78.4%-85.2%, 77.9%-89.0% and 83.0% - 88.1%, respectively. The detection limit of the method was 0.5 ng/g for the target compounds in whole eggs, yolks, and albumens. Finally, the developed method was applied in sulfamethazine analysis of 15 egg samples from Guangzhou City. The results showed that sulfamethazine was detected in only one sample, and the contents of sulfamethazine in whole eggs, yolks, and albumens were 0.66, 0.94, and 0.47 ng/g, respectively. 【Conclusion】 Due to no column chromatography procedure in sample pre-treatment, the method has the advantages of simple operation, low cost and high sensitivity. In addition, this method has good recovery and stability, which is suitable for rapid detection of sulfadimidine in large quantities of whole egg, albumen, and yolk samples.

       

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