一步式固相萃取快速测定动物性食品中氨丙啉残留量
Rapid Determination of Amprolium Residues in Annimal Derived Food Based on One-Step Solid Phase Extraction
薛霞 1宿书芳 1魏莉莉 1卢兰香 1公丕学 1王骏 1刘艳明 1胡梅1
作者信息
- 1. 山东省食品药品检验研究院,国家市场监督重点实验室(肉及肉制品监管技术),产业技术基础公共服务平台,山东济南 250101
- 折叠
摘要
文章建立了一步式固相萃取净化、超高效液相色谱-串联质谱法测定动物性食品中氨丙啉残留量的方法.试样采用80％乙腈溶液(含0.2％甲酸)进行提取,PRiME HLB(Hydrophi liclipophilic balanced)固相萃取柱净化,BEH HILIC(Hydrophilic interaction liquid chromatography)色谱柱分离,乙腈-含0.05％甲酸的5 mmol/L甲酸铵溶液为流动相进行梯度洗脱,电喷雾离子源正离子模式,多反应监测进行检测,基质匹配外标法定量.对提取溶剂、净化方式、色谱柱、流动相组成和质谱参数等重要因素进行了系统的考察.10种基质匹配标准曲线在0.25～100 ng/mL范围内,线性相关系数R2均大于0.99,检出限(Limit of detection,LOD)为2.0 μg/kg,定量限(Limit of quantification,LOQ)为5.0μg/kg.在添加浓度水平5.0、50、500 μg/kg条件下,回收率为86.10％～108.53％,相对标准偏差(n=6)为2.23％～8.42％.该方法采用一步式固相萃取净化,前处理简单、快速,避免溶剂转换、淋洗、洗脱、浓缩等多个处理过程,适用于鸡肉、牛肉、肝脏、肾脏、鸡蛋、脂肪和牛乳等动物性食品中氨丙啉残留的分析测定.
Abstract
A method for the determination of amprolium residues in annimal derived food by ultra-high performance liquid chromatography-tandem mass spectrometry(UHPLC-MS/MS)was established based on one-step solid phase extraction purification.The residues in the test samples were extracted with 80％ acetonitrile solution(containing 0.2％ formic acid),purified by PRiME HLB solid phase extraction column,the samples were analyzed on a BEH HILIC column with a gradient elution using acetonitrile and 5 mmol/L ammonium formate solution containing 0.05％ formic acid as mobile phase.Determination was made in positive ion mode of electrospray ion source by applying multi-reaction monitoring,the samples were quantified with matrix matching external standard method.The important factors such as extraction solvent,purification method,chromatographic column,composition of mobile phase and mass spectrum parameters were investigated systematically.The linear correlation coefficients R2 were all better than 0.99 in the range of 0.25-100 ng/mL for ten kinds of foods.The limit of detection(LOD)was 2.0 μg/kg and the limit of quantification(LOQ)was 5.0 μg/kg in this method.The recoveries from blank foods at three levels of 5,50,500 μg/kg were 86.10％-108.53％ and the relative standard deviations(RSD)(n=6)were 2.23％-8.42％.This method adopts one-step solid phase extraction for purification,making the pretreatment simple and rapid,avoiding multiple processing processes such as solvent conversion,washing,elution and concentration.It is suitable for the analysis and determination of amprolium residues in animal foods such as chicken,beef,liver,kidney,egg,fat and milk.
关键词
一步式固相萃取/氨丙啉/亲水作用/色谱-串联质谱/动物性食品Key words
one-step solid phase extraction/amprolium/hydrophilic action/chromatography-tandem mass spectrometry/annimal derived food引用本文复制引用
基金项目
国家市场监督管理总局科技项目(2022MK072)
出版年
2024
NETL
NSTL
万方数据