UPLC-MS/MS法同时测定不同动物源性食品中硝基呋喃代谢物残留

采用超高效液相色谱串联质谱法(UPLC-MS/MS),建立了猪肉、猪肝、螃蟹和虾4种不同动物源性食品中同时测定4种硝基呋喃类药物代谢物的检测方法,优化了样品前处理的条件以及UPLC-MS/MS仪器条件,样品经盐酸水解,2-硝基苯甲醛衍生,乙酸乙酯提取,ESI正离子模式扫描,多反应监测(MRM)测定。结果表明:采用本方法在4种动物源性样品基质中4种代谢物浓度在1~100 ng/mL范围内线性关系良好;4种代谢物的平均回收率为84.6%~118.1%;相对标准偏差RSD为2.9%~8.1%;在4种样品基质中,3-氨基-2-唑烷基酮(AOZ)的检出限为0.1 μg/kg,定量限为0.4 μg/kg,氨基脲(SEM)和5-甲基吗啉-3-氨基-2-唑烷基酮(AMOZ)的检出限为0.2 μg/kg,定量限为0.5 μg/kg,1-氨基乙内酰脲(AHD)的检出限为0.5 μg/kg,定量限为1.0 μg/kg,均满足国家标准要求。采用本方法对市场上随机购买的80份动物源性样品和鸡肉中硝基呋喃代谢物质控样进行检测,结果与国家标准方法GB/T 20752-2006测定结果相近,质控样的检测结果在量值范围内。该方法前处理操作简便,较传统方法节省时间和成本,可为硝基呋喃类药物残留检测技术提供理论支撑和参考。

Simultaneous Determination of Nitrofuran Metabolite Residues in Different Animal Derived Foods by UPLC-MS/MS

Ultra-performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS) method was developed for the measurement of four metabolites of nitrofuran antibiotics in 4 animal derived foods (porcine muscle, pork liver, crab and shrimp). Samples pretreatment and UPLC-MS/MS conditions were optimized. The samples were hydrolyzed by hydrochloric acid, derivatized by 2-nitrobenzaldehyde, extracted by ethyl acetate, scanned by ESI positive mode and determined by MRM. The results showed that the method had a good linearity within the dynamic range of 1~100 ng/mL. The average recoveries were 84.6%~118.1%, and the relative standard deviations (RSD) were 2.9%~8.1%. The limit of detection (LOD) for 3-amino-2-oxazolidinone (AOZ), semicarbazide (SEM), 5-morpholino-3-amino-2-oxazolidone (AMOZ) and 1-amino-hydantoin (AHD) were 0.1, 0.2, 0.2 and 0.5 μg/kg, respectively. The limit of quantification (LOQ) for 3-amino-2-oxazolidinone (AOZ), semicarbazide (SEM), 5-morpholino-3-amino-2-oxazolidone (AMOZ), and 1-amino-hydantoin (AHD) were 0.4, 0.5, 0.5 and 1.0 μg/kg, respectively, which met the requirements of national standards. The proposed method was used to detect nitrofuran residual in 80 animal derived food samples and quality control samples. The results were close to that detected by national standard method GB/T 20752-2006. The proposed method was time saving and cost-efficient. The results could provide theoretical basis and reference for the detection of nitrofuran residual in animal derived food.