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高效液相色谱-串联质谱法测定鸡蛋中的甲硝唑和地美硝唑

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目的:建立高效液相色谱-串联质谱法测定鸡蛋中甲硝唑和地美硝唑残留的方法.方法:样品依次用乙酸乙酯提取,正己烷除脂,混合阳离子交换固相萃取柱净化后,使用Shimadzu VP-ODS C18 色谱柱分离,以 0.1%甲酸水和 0.1%甲酸乙腈为流动相进行洗脱,多反应监测正离子扫描,外标法定量.结果:甲硝唑和地美硝唑的质量浓度在0~400 μg·L-1 时线性关系良好,检出限和定量限分别为0.5 μg·kg-1 和1.0 μg·kg-1.在 0.5 μg·kg-1、1.0 μg·kg-1、5.0 μg·kg-1 3 个加标水平下,精密度和加标回收率均符合要求.结论:该方法前处理简单、重现性好、回收率高,适用于大批量鸡蛋中甲硝唑、地美硝唑残留的测定.
Determination of Metronidazole and Dimenidazole in Eggs by High-Performance Liquid Chromatography Mass Spectrometry
Objective:To establish a method for the determination of metronidazole and dimenidazole in eggs by high performance liquid chromatography-tandem mass spectrometry.Method:The samples were extracted with ethyl acetate,degreased with n-hexane,and cleaned up with a mixed cation exchange solid phase extraction column.The samples were separated on a Shimadzu VP-ODS C18 column with 0.1%formic acid water and 0.1%formic acid acetonitrile as the mobile phases.Multiple reaction monitoring positive ion scanning and external standard method were used for quantification.Result:The linear relationship between metronidazole and dimenidazole was good in the range of 0~400 μg·L-1,and the limits of detection and quantification were 0.5 μg·kg-1 and 1.0 μg·kg-1,respectively.At the three spiked levels of 0.5 μg·kg-1,1.0 μg·kg-1,and 5.0 μg·kg-1,the precision and spiked recovery rates met the requirements.Conclusion:This method has simple pretreatment,good reproducibility,and high recovery rate,and is suitable for the determination of metronidazole and dimenidazole in large quantities of eggs.

high-performance liquid chromatography mass spectrometryeggsmetronidazoledimenidazole

卢薇、左文婧、丁石花

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宝鸡市食品药品检验检测中心,陕西宝鸡 721000

高效液相色谱-串联质谱法 鸡蛋 甲硝唑 地美硝唑

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.(18)
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