液相色谱—串联质谱技术对食品中主要兽药残留的研究
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摘要
随着人们对食品的质量和安全要求越来越高,近几年来我国发生的食品安全危害事件被频繁报道,一些不法食品生产者和经营者使用违禁药物、超量使用药物剂量、不遵守国家相关法律法规的案件也屡次发生,这为我国食品安全管理人员敲响了警钟,也为我们科研工作者提出了新的要求,如何能够高效、快速、灵敏的检测痕量兽药多残留成为亟待解决的课题。液相色谱串联质谱是食品安全分析的主要技术手段之一,对高沸点、不挥发和热不稳定化合物的分离和鉴定具有独特优势,同时具有多组分的的定性和定量能力,对食品等复杂基质样品中的痕量化合物的测定具有高选择性、高灵敏度的特点。本研究的主要目标是跟踪和瞄准国际上现代残留分析的先进技术,针对食品中主要兽药的残留情况,依据食品中国内外兽药最高残留限量(MRL)要求,通过对食品样品的提取、净化、检测和阳性确证等多方面的系统研究,采用液相色谱-串联质谱技术,建立一系列食品中主要兽药残留的检测方法,并在此研究基础上进行标准化,为我国食品安全状况得到根本改善等诸多方面起到积极重要的作用和奠定下坚实的基础,解决了食品安全检测中的一系列技术难题。本研究分为三个部分,第一部分主要是动物源食品中硝基咪唑类药物残留检测技术研究,第二部分主要是动物源食品中氟喹诺酮类兽药残留检测技术研究,第三部分主要是动物源食品中磺胺类药物残留检测技术研究。通过在对动物源食品样品的提取、净化、检测和阳性确证等多方面的系统研究,研究建立动物源食品中3种主要兽药残留量的系统检测方法,检测的药物品种范围能覆盖和基本满足国内外现行相关法规和标准的要求,检测方法的准确度、精密度满足残留分析质量控制指南的技术要求,检测低限达到国内外MRL的要求,与现行方法相比,整个检验周期缩短50%以上,降低检测成本60%以上,使我国的残留检测技术水平与国际同步。
While the requirements of quality and food safety are changing stricter, the harmful accidents of food safety are frequetly reported, the cases of some immoral producers and sellers of foods using forbidden drugs, overdoing drugs, not observing related legal laws often happen. All these ring alarms for food safety admistrators and propose new requirements for related researchers. How to effectively, quickly, and sensitively determine the trace contents of animal drugs becomes an urgent task. Liquid chromatography tadem mass spectropy (LC-MS/MS) is one of the main food safety analyitcal technologies, which show special advantages to seperation and identification of high boiling point, involatile and Thermo-instable compounds, and high seletivity and sensitivty to trance analysis. The main aim of this research is to follow and target on the morden international residue analysis technolgies. By systemic studying including extraction, cleaningup, determination and positive confirmation etc., using LC-MS/MS, a serial testing methods of determining animal drugs in foods and the followed standardization have been developed, as acts important effect, builds stable base, solve many technical questions for food safety and related areas in China. The research is divided into three parts. The first part is the studying of testing technolgy of nitroimidazoles in animal original foods, the second part is the studying of testing technolgy of fluoroquinolones in animal original foods, the third part is the studying of testing technolgy of sulfonamides in animal original foods. The tested compounds in the yielded methods to determine three animal drugs in animal original foods, cover and satisfy the current domestic and international requirements, the limits of detection conform to the current domestic and international MRL requirements. The testing periods compared to the current mothods are shorten 50%, and the costs are shorten 60%, as makes the residue analysis of China step the same pace as the internation level.
引文
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