高效液相色谱-串联质谱法快速测定鸡蛋中的甲硝唑  

Rapid Determination of Metronidazole in Egg by UPLC-MS/MS

作　　者：张金磊 邢丽杰[1] 罗瑞峰[1] 张飞 陈永发 巩婧婷 贺玉凤[1] ZHANG Jinlei;XING Lijie;LUO Ruifeng;ZHANG Fei;CHEN Yongfa;GONG Jingting;HE Yufeng(Analysis and Testing Center,Xinjiang Academy of Agriculture and Reclamation Science,Shihezi,Xinjiang 832000,China)

机构地区：[1]新疆农垦科学院分析测试中心,新疆石河子832000

出　　处：《农产品加工》2022年第22期49-51,55,共4页Farm Products Processing

摘　　要：建立了鸡蛋中甲硝唑的高效液相色谱-串联质谱(UPLC-MS/MS)快速分析测定方法。样品经0.2%甲酸乙腈超声提取,用PRiME HLB固相萃取小柱净化,甲醇-水梯度洗脱,色谱柱(ZORBAX SB-Aq Solvent Saver Plus,3.0 mm×100 mm,3.5μm)分离,采用多反应监测(MRM)正离子模式对鸡蛋中甲硝唑进行测定,基质匹配标准曲线外标法定量。结果表明,在优化条件下,甲硝唑在0~40 ng/mL质量浓度范围内均呈现良好的线性关系(R^(2)=0.9996),检出限为0.5μg/kg,定量限为1.0μg/kg。在鸡蛋样品中进行3个水平的添加试验(n=6),平均回收率为83.2%~104.0%,相对标准偏差0.8%~1.2%。表明该方法适用于鸡蛋样品中甲硝唑的测定。A rapid method for the determination of metronidazole in eggs by High-performance liquid chromatography tandem mass spectrometry(UPLC-MS/MS)was established.The sample was extracted with 0.2%formic acid acetonitrile by ultrasound,purified with PRiME HLB solid phase extraction(SPE),eluted with methanol-water gradient,and separated by chromatography(3.0 mm×100 mm,3.5μm),metronidazole in eggs was determined by Multiple Reaction Monitoring(MRM)positive ion mode,and the matrix matching standard curve was used for external standard determination.The results showed that metronidazole showed a good linear relationship in the concentration range of 0~40 ng/mL(R^(2)=0.9996).The detection limit was 0.5μg/kg and the quantitative limit was 1.0μg/kg.The average recovery was 83.2%~104.0%and the relative standard deviation was 0.8%~1.2%.The results showed that the method was suitable for the determination of metronidazole in egg samples.

关 键 词：甲硝唑 高效液相色谱-串联质谱法(UPLC-MS/MS) 鸡蛋 

分 类 号：R155[医药卫生—营养与食品卫生学]