一种生物相容性固相萃取技术及初步应用研究

发布时间：2019-06-15 06:06

【摘要】：食品的安全问题是关乎人的生命健康的重大问题,它依赖于从生产源头到销售的各个环节。不仅需要相关的法律来规范食品的生产、运输和销售等方面,而且还需不断提高分析手段来控制食物的品质。在动物源食品的兽药残留分析中,复杂样品基质带来的干扰是面临的主要难题,开发具有良好生物相容性样品前处理技术是兽药残留分析工作的关键。本实验采用改性的固相萃取柱对猪肉样品中的盐酸克伦特罗进行了提取,并用HPLC法分离检测。具体研究内容分为两个部分。第一部分SDS改性固相萃取柱-HPLC法测定猪肉中的盐酸克伦特罗目的:简化样品前处理步骤,实现从猪肉的酸性匀浆液中直接提取克伦特罗,并用HPLC分离检测。方法:采用经表面活性剂SDS动态改性的C18固相萃取柱,富集净化猪肉样品中的盐酸克伦特罗,再经HPLC分离检测。结果:该方法在0.1~10.0mg/kg浓度范围内具有良好的线性关系,相关系数R2=0.9989;3个浓度水平的方法回收率在96.36%~103.96%之间,RSD(n=5)在4.46%~5.10%范围内;检测限(S/N=3)为20.0μg/kg。结论:本实验所建立的方法具有快速、简便、准确等特点,成功用于动物源食品中盐酸克伦特罗的选择性富集净化和分离检测,并且有望用于其它含有疏水母核的碱性兽药的提取分析。第二部分Tween-20改性固相萃取柱-HPLC法测定猪肉中的盐酸克伦特罗目的:从动物源食品中有效萃取克伦特罗的同时,能显著降低动物食品样品基质中蛋白质等大分子带来的干扰和污染。方法:采用一定量的非离子型中性表面活性剂Tween-20对C18固相萃取柱进行动态改性,形成亲水性表面,富集净化猪肉中的克伦特罗,再经HPLC分离检测猪肉样品中的盐酸克仑特罗。结果:分析结果表明,该方法在0.2~10.0mg/kg添加浓度内呈良好的线性关系,相关系数R2=0.9986;3个添加浓度(5.0mg/kg,1.0mg/kg,0.5mg/kg)回收率在96.07%~107.75%之间;RSD(n=5)在2.27%~3.51%之间;检测限(S/N=3)为25.0μg/kg。结论:本实验经非离子型中性表面活性剂Tween-20动态改性的C18固相萃取柱,具有良好的表面亲水性,对蛋白质等大分子具有屏蔽和排阻作用,可以降低复杂基质带来干扰,并有效地富集净化盐酸克仑特罗。这是一种生物相容性固相萃取技术,具有简便、高效和成本低等特点,可广泛应用于动物源食品中的兽药残留分析。
[Abstract]:Food safety is a major issue related to human life and health, which depends on every link from the source of production to the sale. Not only the relevant laws are needed to regulate the production, transportation and sale of food, but also analytical methods are needed to control the quality of food. In the analysis of veterinary drug residues in animal food, the interference caused by complex sample matrix is the main problem. The development of pretreatment technology of samples with good biocompatibility is the key to the analysis of veterinary drug residues. In this experiment, clenbuterol hydrochloric acid in pork samples was extracted by modified solid phase extraction column and separated and detected by HPLC. The specific research content is divided into two parts. Part 1 determination of Clenbuterol Hydrochloride in Pork by SDS modified solid Phase extraction column-HPLC objective: to simplify the pretreatment steps of samples, to extract clenbuterol directly from acid homogenate of pork, and to separate and detect clenbuterol by HPLC. Methods: C 18 solid phase extraction column modified by surfactants SDS was used to enrich and purify clenbuterol hydrochloric acid in pork samples, and then separated and detected by HPLC. Results: the method had a good linear relationship in the range of 0.1~10.0mg/kg concentration. The recovery of the method was 96.36% 鈮，

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