液相色谱-串联质谱测定鸡蛋中4种硝基呋喃类代谢物残留

Determination of Four Metabolite Residues of Nitrofuran Antibiotics in Eggs by Liquid Chromatography-tande mmol/Lass Spectrometry

[目的]建立一种测定鸡蛋中硝基呋喃类代谢物残留的液相色谱-串联质谱法。[方法]样品经在酸性条件下水解,加入衍生试剂2-硝基苯甲醛,37℃避光孵育16 h,Na 2EDTA-McⅡ-vaine缓冲溶液和乙酸乙酯共同提取,经固相萃取去除基质中的干扰物,液相色谱-串联质谱进行检测。[结果]4种兽药残留采用同位素内标法定量,在0.1~20.0μg/kg线性关系良好,相关系数均大于0.99,方法回收率为79.85%~102.17%,相对标准偏差(RSD)为1.64%~9.16%,定量限为0.5μg/kg。[结论]该方法前处理相对简单、准确且灵敏度高,适用于鸡蛋中4种硝基呋喃类代谢物药物残留检测。

[Objective]The research aimed to establish a liquid chromatography-tandem mass spectrometry method for the determination of nitrofuran metabolite residues in eggs.[Method]The sample was hydrolyzed under acidic conditions,and the derivatizing reagent 2-nitrobenzaldehyde was added.The mixture was incubated at 37℃for 16 h in the dark.The Na2EDTA-McII-vaine buffer solution and ethyl acetate were co-extracted,the interfering substances in the matrix were removed by solid phase extraction and detected by liquid chromatography-tandem mass spectrometry.[Result]The residues of the four veterinary drugs were quantified by isotope internal standard method.The linear relationship was good at 0.1-20.0μg/kg,the correlation coefficient was greater than 0.99,the recovery rate was 79.85%-102.17%,and the relative standard deviation(RSD)was 1.64%-9.16%.The limit of quantification is 0.5μg/kg.[Conclusion]The method is relatively simple,accurate and sensitive,and is suitable for the detection of four nitrofuran metabolites in eggs.