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目的建立动物源性食品中四种硝基呋喃代谢物的超高效液相色谱串联质谱(ultra pressure liquid chromatography-tandem mass spectrometry,UPLC-MS/MS)的快速检测方法。方法样品经盐酸溶液水解,邻硝基苯甲醛(2-NBA)37℃衍生16 h后,调节衍生液的pH=7.6,用乙酸乙酯提取。分析物采用电喷雾电离,正离子扫描,多反应检测模式(MRM),基质匹配内标标准曲线法定量。结果四种代谢物的工作曲线在0.1～10.0μg/L浓度范围内线性良好,相关系数R2均达到了0.995以上,氨基脲(SEM或SCA)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。平均回收率在91.8%～107.0%之间,相对标准偏差均小于10%。结论样品前处理简单、测定时间短、灵敏度高,适用于猪肉、牛肉、鸡肉、猪肝和水产品(鱼类及虾类)中硝基呋喃类代谢物残留的快速测定。
Objective To establish a rapid method for the determination of four nitrofuran metabolites in animal derived foods by ultra pressure liquid chromatography-tandem mass spectrometry (UPLC-MS / MS). Methods The samples were hydrolyzed with hydrochloric acid solution and o-nitrobenzaldehyde (2-NBA) was derivatized at 37 ℃ for 16 h. The pH of derivative solution was adjusted to 7.6 and extracted with ethyl acetate. The analytes were quantified by electrospray ionization, positive ion scanning, multi-reaction detection mode (MRM), and matrix matching internal standard curve method. Results The calibration curves of the four metabolites showed a good linearity in the concentration range of 0.1-10.0 μg / L, the correlation coefficients R2 reached above 0.995, and SEM and SCA and 1-amino-hydantoin (AHD) were the lowest The detection limits were 0.1μg / kg. The detection limits of 5-morpholinomethyl-3-amino-2-oxazolidinone (AMOZ) and 3-amino- 0.05μg / kg. The average recoveries ranged from 91.8% to 107.0% with relative standard deviations less than 10%. Conclusion The sample pretreatment is simple, the measurement time is short, and the sensitivity is high. It is suitable for the rapid determination of nitrofuran metabolites residues in pork, beef, chicken, liver and aquatic products (fish and shrimp).