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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 To establish a method for the simultaneous determination of four nitrofuran metabolites in eggs by ultra high pressure liquid chromatography-tandem mass spectrometry (UPLC-MS / MS). Methods Hydrolysis of the protein-bound nitrofuran metabolites in eggs with o-nitrobenzaldehyde (2-NBA) yielded stable derivatives extracted with ethyl acetate and centrifuged at 4 ° C. The clarified Liquid determination. The analyte is electrospray ionized positive ion, multi-reaction monitoring mode detection, matrix internal standard quantification. Results The concentrations of four analytes showed a good linear relationship with the peak area ratio in the range of 0.1-50.0 μg / L with the correlation coefficients of no less than 0.995. The recoveries ranged from 74.1% to 97.6% with a RSD of 13.4%. The detection limits of semicarbazide (SEM) and 1-amino-hydantoin (AHD) were both 0.1μg / kg. The lowest detection limits of 5-morpholinomethyl-3-amino-2-oxazolidinone (AMOZ) The detection limits of 3-amino-2-oxazolidinone (AOZ) were both 0.05μg / kg. Conclusion The method has the advantages of simple sample pretreatment, high sensitivity and good reproducibility, and meets the requirements of quantitative detection of four kinds of metabolites of nitrofuran in eggs.