超高效液相色谱串联质谱法测定动物源食品中4种硝基呋喃代谢物  

Determination of Four Nitrofuran Metabolites in Animal Derived Food by Ultra-High Performance Liquid Chromatography Tandem Mass Spectrometry

作　　者：边文科 王润昊 BIAN Wenke;WANG Runhao(College of Agricultural Engineering and Food Science,Shandong University of Technology,Zibo 255049,China;Shandong Burey Inspection and Testing Co.,Ltd.,Zibo 256400,China)

机构地区：[1]山东理工大学农业工程与食品科学学院,山东淄博255049 [2]山东博锐检验检测有限公司,山东淄博256400

出　　处：《食品安全导刊》2024年第22期69-76,共8页China Food Safety Magazine

摘　　要：本研究建立了超高效液相色谱串联质谱法同时检测动物源食品中3-氨基-2-噁唑烷基酮(3-Amino-2-Oxazolidinone,AOZ)、5-吗啉甲基-3-氨基-2-噁唑烷基酮(3-Amino-5-Morpholinomethyl-2-Oxazolidinone,AMOZ)、氨基脲(Semicarbazide,SEM)、1-氨基-2-内酰脲(1-Aminohydantoin,AHD)残留量的分析方法。样品以0.2 mol·L^(-1)盐酸水为提取剂,加入2-硝基苯甲醛为衍生剂,37℃水浴振荡4 h,调节pH值为7.4±0.2,HLB固相萃取柱净化,氮气吹干,用0.1%甲酸(含有50%甲醇)水溶液复溶,采用0.1%甲酸水-10 mmol·L^(-1)乙酸铵和甲醇为流动相梯度洗脱,经C_(18)柱分离,电喷雾正离子模式扫描,多反应监测模式,内标法定量。结果表明,4种硝基呋喃药物线性良好,相关系数(R^(2))均大于0.999,动物源食品中AOZ、AMOZ、SEM、AHD的检出限均为0.2μg·kg^(-1),定量限为0.4μg·kg^(-1)。低、中、高浓度加标水平下,4种化合物在畜肉产品中的回收率为87.42%~102.26%,相对标准偏差为0.80%~5.93%;在禽肉产品中的回收率为89.76%~104.94%,相对标准偏差为0.62%~5.83%;在禽蛋产品中的回收率为90.30%~106.82%,相对标准偏差为0.85%~7.93%;在水产品中的回收率为86.95%~107.36%,相对标准偏差为0.20%~5.02%。该方法灵敏度高、重复性好,可为实验室大批量检测动物源食品中硝基呋喃类药物提供技术参考。In this research,an ultra-high performance liquid chromatography tandem mass spectrometry(UPLC-MS/MS) was developed for the simultaneous determination of 3-amino-2-oxazolidinone (AOZ),5-morpholinomethyl-3-amino-2-oxazolidinone (AMOZ),semicarbazide (SEM) and 1-aminohydontion (AHD)residues in food from animal origin.These samples were treated with 0.2 mol·L^(-1) hydrochloric acid water as an extract and 2-nitrobenzaldehyde as derivative.Samples were shaken in a water bath at 37℃for 4 h,and the pH was adjusted to 7.4±0.2,and purified by HLB solid phase extraction column,then dried by nitrogen,used 0.1%formic acid water to redissolve (included 50%methanol),0.1%formic acid water are mixed with 10 mmol·L^(-1) ammonium acetate and methanol as mobile phase to gradient.C_(18) column to separation,scanning electrospray positive in ion mode and multi-reaction monitoring mode,quantification by internal standards.The results showed that the four nitrofuran drugs had good linearity,and correlation coefficients (R^(2)) were all greater than 0.999.The detection limits of AOZ,AMOZ,SEM and AHD in animal food were all 0.2μg·kg^(-1),and quantitation limits were 0.4μg·kg^(-1).At low,medium and high concentration addition levels,the recovery rates of the four compounds in livestock meat products were 87.42%~102.26%,and the relative standard deviations were 0.8%~5.93%;the recovery rates in poultry meat products were 89.76%~104.94%,the relative standard deviations were 0.62%~5.83%;the recovery rates in poultry egg products were 90.30%~106.82%,the relative standard deviations were 0.85%~7.93%;the recovery rates in aquatic products were 86.95%~107.36%,and the relative standard deviations were 0.20%~5.02%.The the method has high sensitivity and good repeatability,which providing technical reference for the detection of nitrofurans in large quantities of animal food in laboratory.

关 键 词：超高效液相色谱串联质谱 动物源食品 硝基呋喃类药物 

分 类 号：O657.63[理学—分析化学] TS207.3[理学—化学]