超高压液相色谱-串联质谱法同时测定鸡蛋中4种硝基呋喃代谢物残留

Determination of four nitrofuran residues in eggsusingultra pressure liquid chromatography-tandem mass spectrometry

目的建立超高压液相色谱-串联质谱法（UPLC-MS/MS）同时测定鸡蛋中4种硝基呋喃代谢物的方法。方法鸡蛋中与蛋白质结合的硝基呋喃代谢物经盐酸水解后,与邻硝基苯甲醛（2-NBA）反应,产生稳定的衍生物,用乙酸乙酯提取,4℃冷冻离心后取下层澄清液测定。待测物采用电喷雾电离正离子、多反应监测模式检测,基质内标法定量。结果4种待测物浓度在0.1~50.0μg/L范围内与其峰面积比值呈良好的线性关系,相关系数均不低于0.995,回收率范围为74.1%~97.6%,RSD〈13.4%。氨基脲（SEM）与1-氨基-乙内酰脲（AHD）最低检出限均为0.1μg/kg,5-吗啉甲基-3-氨基-2-恶唑烷基酮（AMOZ）与3-氨基-2-恶唑烷基酮（AOZ）最低检出限均为0.05μg/kg。结论该方法具有样品前处理简单、灵敏度高、重现性好等优点,满足鸡蛋中4种硝基呋喃代谢物残留定量检测的要求。

Objective A rapid analytical method for the simultaneous detection of four metabolites of nitrofuran in eggs by the ultra pressure liquid chromatography-tandem mass spectrometry （UPLC-MS/MS） was established. Methods The metabolites in egg samples were released in HC1 solution, and reacted with the 2-nitrob6nzaldehyde （2-NBA）. The stable derivatives were extracted by ethyl acetate, and centrifuged at. The transparent liquid was detected. The identification was achieved by electro spray ionization in positiw mode using multiple reaction monitoring. The quantification was performed by the matrix matched internal standards. Results The calibration curves of the four analytes showed a good linearity between 0. 1 and 50μg/L, and the correlation coefficient was above 0. 995. Recoveries were between 74. 1% and 97.6% with RSD less than 13.4%. The limits of detection of SEM and AHD were 0. 1 μg/kg, and the limits of detection of AMOZ and AOZ were 0.05 μg/kg. Conclusion The method has the advantages of simple pretreatment, high sensitivity and good reproducibility, which is suitable for the determination of four nitrofuran metabolites in eggs.