猪的四种组织中巴氯芬的定量确证方法

发布时间：2018-12-31 10:01

【摘要】：随着人们对动物源性食品的安全和质量要求越来越高,健康环保养殖将成为一种趋势,近年来在食品动物的饲养过程中不合理用药和非法添加违禁药物,以及不遵守休药期规定等现象,使这些问题食品的危害逐渐增加,这对我们从事食品研究和检测相关行业的科研工作者提出了更高的要求,如何简便、灵敏、高效的检测兽药残留问题成为摆在我们面前的首要难题。液相色谱串联质谱(LC-MS/MS)是食品安全、药物残留分析的主要技术手段之一,对于不挥发、热不稳定、高沸点化合物的鉴定与分离具有独特的优势,对于基质相对复杂的样品具有高灵敏度、高选择性等特点。巴氯芬由一个氯苯基和一个羧基以及一个氨基组成,所以具有酸碱两性,易溶于水和急性有机溶剂。巴氯芬是β-受体兴奋剂,因此禁止用做添加剂使用,由于其具有营养再分配作用,能够有效提高瘦肉产量,因此可被当做盐酸克伦特罗替代品用于动物的养殖当中,有必要开发方法对其残留物进行检测,防止不法分子在动物养殖中使用。然而,一些方法已被报道用于巴氯芬在动物的尿液和肌肉的残留分析。那么,这项工作的目的是建立一个相对敏感的LC-MS/MS确证法检测巴氯芬残留在猪肝脏,肾脏,肌肉,脂肪的含量。所采用的方法是在酸水解后,将样品用异丙醇-乙酸乙酯提取(4：6),蒸干后复溶过SPE并收集,收集液最后蒸发至干并重新溶解在水/甲醇混合物中,通过LC-MS/MS进行测定。使用选择反应监测(SRM)正离子检测巴氯芬。该方法肝脏,肾脏,肌肉和脂肪的定量限分别为1.0,1.0,1.0和1.0微克/千克。该方法根据欧盟委员会2002/657/EC决议对线性,正确度,精密度,特异性,CCα,CCβ进行了验证。所有的正确度值保持在88.4和94.1%之间。各级测试浓度的精确度值具有优良的相对标准偏差(RSD15%)。该方法在每种组织中的CCα和CCβ值已经建立。该方法适用于检测巴氯芬在猪的四种组织中的残留。
[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 伪 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 伪 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.
【学位授予单位】：湖南农业大学
【学位级别】：硕士
【学位授予年份】：2015
【分类号】：S859.84

【相似文献】