【摘要】：隨著人們對動物源性食品的安全和質(zhì)量要求越來越高,健康環(huán)保養(yǎng)殖將成為一種趨勢,近年來在食品動物的飼養(yǎng)過程中不合理用藥和非法添加違禁藥物,以及不遵守休藥期規(guī)定等現(xiàn)象,使這些問題食品的危害逐漸增加,這對我們從事食品研究和檢測相關(guān)行業(yè)的科研工作者提出了更高的要求,如何簡便、靈敏、高效的檢測獸藥殘留問題成為擺在我們面前的首要難題。液相色譜串聯(lián)質(zhì)譜(LC-MS/MS)是食品安全、藥物殘留分析的主要技術(shù)手段之一,對于不揮發(fā)、熱不穩(wěn)定、高沸點化合物的鑒定與分離具有獨特的優(yōu)勢,對于基質(zhì)相對復(fù)雜的樣品具有高靈敏度、高選擇性等特點。巴氯芬由一個氯苯基和一個羧基以及一個氨基組成,所以具有酸堿兩性,易溶于水和急性有機溶劑。巴氯芬是β-受體興奮劑,因此禁止用做添加劑使用,由于其具有營養(yǎng)再分配作用,能夠有效提高瘦肉產(chǎn)量,因此可被當做鹽酸克倫特羅替代品用于動物的養(yǎng)殖當中,有必要開發(fā)方法對其殘留物進行檢測,防止不法分子在動物養(yǎng)殖中使用。然而,一些方法已被報道用于巴氯芬在動物的尿液和肌肉的殘留分析。那么,這項工作的目的是建立一個相對敏感的LC-MS/MS確證法檢測巴氯芬殘留在豬肝臟,腎臟,肌肉,脂肪的含量。所采用的方法是在酸水解后,將樣品用異丙醇-乙酸乙酯提取(4：6),蒸干后復(fù)溶過SPE并收集,收集液最后蒸發(fā)至干并重新溶解在水/甲醇混合物中,通過LC-MS/MS進行測定。使用選擇反應(yīng)監(jiān)測(SRM)正離子檢測巴氯芬。該方法肝臟,腎臟,肌肉和脂肪的定量限分別為1.0,1.0,1.0和1.0微克/千克。該方法根據(jù)歐盟委員會2002/657/EC決議對線性,正確度,精密度,特異性,CCα,CCβ進行了驗證。所有的正確度值保持在88.4和94.1%之間。各級測試濃度的精確度值具有優(yōu)良的相對標準偏差(RSD15%)。該方法在每種組織中的CCα和CCβ值已經(jīng)建立。該方法適用于檢測巴氯芬在豬的四種組織中的殘留。
[Abstract]:With the increasing demands on the safety and quality of animal-derived food, healthy and environmentally friendly breeding will become a trend. In recent years, irrational use of drugs and illegal addition of illegal drugs have been used in the process of food and animal breeding. As well as the phenomenon of not complying with the regulations on the withdrawal period, the harm caused by these problem foods has gradually increased. This has put forward higher requirements for our scientific research workers engaged in food research and testing related industries, how to be simple and sensitive, Efficient detection of veterinary drug residues has become the most important problem in front of us. Liquid chromatography-tandem mass spectrometry (LC-MS/MS) is one of the main techniques for food safety and drug residue analysis. It has unique advantages in the identification and separation of non-volatile, heat-unstable and high-boiling compounds. The samples with relatively complex matrix have the characteristics of high sensitivity, high selectivity and so on. Baclofen is composed of a chlorophenyl group, a carboxyl group and an amino group, so it is acid-base amphoteric, easily soluble in water and in acute organic solvents. Baclofen is a beta-receptor stimulant and is therefore prohibited from being used as an additive. Because of its nutritional redistribution, it can effectively increase lean meat production and can therefore be used as an alternative to clenbuterol hydrochloride in animal breeding. It is necessary to develop methods to detect its residues to prevent illegal elements from being used in animal breeding. However, some methods have been reported for analysis of baclofen residues in urine and muscle in animals. The aim of the work was to establish a relatively sensitive LC-MS/MS assay for the detection of baclofen residues in the liver, kidney, muscle, and fat of pigs. After acid hydrolysis, the sample was extracted with isopropyl alcohol-ethyl acetate (4:6), then evaporated into SPE and collected. The collection solution was evaporated to dry and dissolved again in the water / methanol mixture. The results were determined by LC-MS/MS. The selective reaction was used to monitor (SRM) positive ions for the detection of baclofen. The quantitative limits of liver, kidney, muscle and fat were 1.0 渭 g / kg and 1.0 渭 g / kg, respectively. The linearity, accuracy, precision, specificity, CC 偽 and CC 尾 of the method were verified according to the 2002/657/EC resolution of the European Commission. All accuracy values remained between 88.4 and 94.1%. The accuracy values of each test concentration have excellent relative standard deviation (RSD15%). The CC 偽 and CC 尾 values in each tissue have been established. This method is suitable for the detection of baclofen residues in four tissues of pigs.
【學(xué)位授予單位】：湖南農(nóng)業(yè)大學(xué)
【學(xué)位級別】：碩士
【學(xué)位授予年份】：2015
【分類號】：S859.84

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