摘要
建立液相色谱-串联质谱(liquid chromatography-tandem mass spectrometry,LC-MS/MS)法测定鸡蛋、鸡肉和蛋糕中氟虫腈及其代谢物残留量的方法。样品经酸性乙腈提取,经Cleanert PEP Plus(60 mg/3 m L)固相萃取柱净化,Agilent Eclipse plus C18色谱柱(2.1 mm×100 mm,1.8μm)分离,以0.1%甲酸乙腈溶液和0.1%甲酸水溶液(含10 mmol/L乙酸铵)为流动相进行梯度洗脱,电喷雾负离子模式电离,多反应监测模式检测,外标法定量。对鸡蛋、鸡肉和蛋糕3种基质效应进行了试验。结果表明1μg/kg～50μg/kg范围内线性关系良好,相关系数R2>0.99。方法的检出限为0.4μg/kg,定量限为1μg/kg。在鸡蛋、鸡肉和蛋糕中分别添加1、2、5μg/kg 3个水平进行加标回收试验,回收率为82.3%～112.5%,相对标准偏差为1.2%～4.5%。该方法具有较高的灵敏度和准确度,适用于鸡蛋、鸡肉和蛋糕中氟虫腈及残留物的测定。
A liquid chromatography-tandem mass spectrometry (LC-MS/MS) was established for the determination of fipronil and its metabolites in egg ,chicken and cake . The samples were extracted with acid-acetonitrile,cleaned up by Cleanert PEP Plus(60 mg/3 mL). The separation was performed on an Agilent Eclipse plus -C18 column (2.1 mm×100 mm,1.8 μm) with the mobile phases of 10 mmol/L ammonium acetate aqueous solution containing 0.1 % formic acid and acetonitrile containing 0.1 % formic acid. The identification and quantitation of fipronil and its metabolites were performed by MS/MS in negative electrospray ionization (ESI-) and multiple reaction monitoring (MRM) mode. The quantitative analysis was carried out by external standard method. Three matrixes containing egg,chicken and cake were experimented. A good linear relationship,with the correlation coefficient (R2) greater than 0.99,was found in the mass concentration range of 1 μg/kg-50 μg/kg. The limit of detection and limit of quantitation were 0.4 μg/kg and 1 μg/kg respectively. The recoveries of fipronil and its metabolites in different matrixes spiked with 1,2,5 μg/kg varied from 82.3 % to 112.5 %,and the relative standard deviations were between 1.2 % and 4.5 %. The method is sensitive,accurate and suitable for the monitoring of fipronil and its metabolites.
作者
王永芳
王利强
温华蔚
WANG Yong-fang;WANG Li-qiang;WEN Hua-wei(Animal,Plant and Foodstuffs Inspection Center,Tianjin Customs,Tianjin 300461,China)
出处
《食品研究与开发》
CAS
北大核心
2019年第10期163-169,共7页
Food Research and Development
基金
天津检验检疫科技计划项目(TK009-2017)
作者简介
王永芳(1985-),女(汉),工程师,硕士,研究方向:食品中农药残留检测。
