液相色谱串联质谱在聚醚类兽药残留分析中的应用研究

发布时间：2018-11-07 13:53

【摘要】：近些年来,食品污染越来越成为人们关注的焦点,其中以兽药残留引起的为代表。兽药是水产养殖业和畜牧业中非常重要的一部分,但不合理,乱用,滥用导致的兽药残留危害这人类健康的同时也影响着国际间的贸易。动物源样品大多存在这基质复杂,干扰多的问题,因此简单有效的净化手段很有必要,对于测定这些痕量残留工作,SPE为较好的前处理手段,它可以实现从复杂的基质中提取出来痕量目标物,也可以起到净化,富集和浓缩的作用,本文研究了动物源食品中6种聚醚类抗生素的检测,采用了高灵敏度、高选择性、极强专属性的液相色谱-串联质谱进行分析。本论文主要研究内容如下:第一章:综述了课题背景及意义,固相萃取前处理方法及在线净化前处理方法,质谱原理与液相色谱串联质谱简述。第二章:建立了固相萃取液相色谱串联质谱法测定动物源食品中聚醚类抗生素的残留。比较3类5种固相萃取柱,通过比较其基质应用范围,基质效应及操作性,确定了石墨化炭黑固相萃取柱作为净化柱,该方法适用于牛奶,鸡肉,鸡蛋,鸡肝4种动物源性基质,方法简便,灵敏度高,重现性好。第三章:建立了在线净化液相色谱串联质谱法快速测定动物源性食品中聚醚类抗生素,使用了TurboFlow在线净化液相色谱串联质谱联用技术实现了6种聚醚类抗生素的同时分析,简化了前处理步骤,实现了样品净化、富集和分析的自动化,方法的技术指标满足国内相关法规的要求。
[Abstract]:In recent years, food pollution has become the focus of attention, among which veterinary drug residue is the representative. Veterinary medicine is a very important part of aquaculture and animal husbandry, but unreasonable, indiscriminate use, misuse of veterinary drug residues that harm human health, but also affect the international trade. Most of the animal samples have the problems of complex matrix and many interference, so it is necessary to use simple and effective purification methods. SPE is a good pretreatment method for the determination of these trace residues. It can be used to extract trace target from complex matrix, but also to purify, enrich and concentrate. In this paper, six kinds of polyether antibiotics in animal food were detected with high sensitivity and selectivity. Highly specific liquid chromatography-tandem mass spectrometry (LC-MS) was used for analysis. The main contents of this thesis are as follows: in chapter 1, the background and significance of the research, the pretreatment methods of solid phase extraction and on-line purification, the principle of mass spectrometry and the tandem mass spectrometry of liquid chromatography are reviewed. Chapter 2: solid phase extraction liquid chromatography tandem mass spectrometry was established for the determination of polyether antibiotics in animal food. By comparing three kinds of five kinds of solid phase extraction (SPE) columns, by comparing their application scope, matrix effect and operation, the graphitized carbon black solid-phase extraction column was determined as purification column. The method is suitable for milk, chicken and egg. The method is simple, sensitive and reproducible. Chapter 3: the rapid determination of polyether antibiotics in animal food by on-line purification liquid chromatography-tandem mass spectrometry was established. Six polyether antibiotics were analyzed simultaneously by TurboFlow on-line purification liquid chromatography-tandem mass spectrometry. The pretreatment process is simplified, and the automation of sample purification, enrichment and analysis is realized. The technical specifications of the method meet the requirements of relevant domestic laws and regulations.
【学位授予单位】：河北科技大学
【学位级别】：硕士
【学位授予年份】：2015
【分类号】：S859.84

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