CAJ | 학술논문

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。
목적：건립동물원성식품중사충초기부남대사물적초고효액상색보천련질보(ultra pressure liquid chromatography-tandem mass spectrometry, UPLC-MS/MS)적쾌속검측방법。방법양품경염산용액수해,린초기분갑철(2-NBA)37℃연생16 h후,조절연생액적pH=7.6,용을산을지제취。분석물채용전분무전리,정리자소묘,다반응검측모식(MRM),기질필배내표표준곡선법정량。결과사충대사물적공작곡선재0.1～10.0μg/L농도범위내선성량호,상관계수R2균체도료0.995이상,안기뇨(SEM혹SCA)여1-안기-을내선뇨(AHD)최저검출한균위0.1μg/kg,5-마람갑기-3-안기-2-악서완기동(AMOZ)여3-안기-2-악서완기동(AOZ)최저검출한균위0.05μg/kg。평균회수솔재91.8%～107.0%지간,상대표준편차균소우10%。결론양품전처리간단、측정시간단、령민도고,괄용우저육、우육、계육、저간화수산품(어류급하류)중초기부남류대사물잔류적쾌속측정。
Objective A rapid analytical method for the detection of metabolites of nitrofuran in food by the ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) was established. Methods The metabolites in food samples were released in HCl solution, and derived using 2-nitrobenzaldehyde (2-NBA) at 37 ℃ for 16 h. The pH values of derivates were adjusted to 7.6, and then the analytes were extracted by ethyl acetate. Identification was achieved by electrospray ionization in posi-tive mode (ESI+) using multiple reaction monitoring (MRM). The quantification was performed by the ma-trix matched internal standards. Results The calibration curves of the four analytes showed a good linearity in the concentrations of 0.1～10μg/L with R2 above 0.995. The limits of detection of SCA and AHD were 0.1μg/kg, and the limits of detection of AMOZ and AOZ were 0.05μg/kg. Recoveries were between 91.8%and 107.0%with the relative standard deviations (RSD) less than 10%. Conclusion This method simplifies the sample pre-treatment, and reduces the detection time, and it is a fast, highly selective and sensitive assay. The method can apply to the rapid detection of nitrofuran metabolites in pork, beef, chicken, porcine liver, fish and shrimp.