首页|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

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

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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C18 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(R2)均大于 0.999,动物源食品中AOZ、AMOZ、SEM、AHD的检出限均为 0.2 μg·kg-1,定量限为 0.4 μg·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.
Determination of Four Nitrofuran Metabolites in Animal Derived Food by Ultra-High Performance Liquid Chromatography Tandem Mass Spectrometry
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.C18 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(R2)were all greater than 0.999.The detection limits of AOZ,AMOZ,SEM and AHD in animal food were all 0.2 μg·kg-1,and quantitation limits were 0.4 μg·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.

ultra high performance liquid chromatography tandem mass spectrometryanimal derived foodnitrofuran drugs

边文科、王润昊

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山东理工大学 农业工程与食品科学学院,山东淄博 255049

山东博锐检验检测有限公司,山东淄博 256400

超高效液相色谱串联质谱 动物源食品 硝基呋喃类药物

2024

食品安全导刊
商业科技质量中心 北京肉类食品协会

食品安全导刊

影响因子:0.065
ISSN:1674-0270
年,卷(期):2024.(22)