动物组织中硝基呋喃代谢物残留量的测定方法---食品科学与工程毕业论文.docVIP

山东理工大学 毕业论文 题 目：动物组织中硝基呋喃代谢物残 留量的测定方法 学 院： 专 业： 食品科学与工程 学生姓名： 指导教师： 毕业论文时间：二ОО八年二月二十五日～六月二十日 共十七周  摘 要 用高效液相色谱-串联质谱（LC-MS/MS）法同时测定动物组织及水产品中呋喃唑酮、呋喃它酮、呋喃西林和呋喃妥因的代谢物。盐酸水解动物组织及水产品中蛋白结合的代谢物，同时加入2-硝基苯甲醛（2-NBA），37℃过夜衍生化。加入氢氧化钠，调节PH值至7.0后，再加入正己烷去除蛋白。后用乙酸乙酯提取，正己烷净化，分析物采用电喷雾电离正离子（ESI+）、多反应检测（MRM）模式检测，內标法定量。在添加浓度0.5~2μg/kg范围内，內标法回收率为89.5%~110.3%；相对标准偏差（RSD）小于11.3%。5-马啉代甲基-3-氨基-2-恶唑酮（5-methylmorpholino-3-amino-2-oxazolidinone，AMOZ）、3-氨基-2-恶唑酮（3-amino-2-oxazolidinone，AOZ）、氨基脲（semicarbazide，SEM）和1-氨基-乙内酰胺（1-amino-hydantoin，AHD）方法检出限为0.5μg/kg。 关键词：液相色谱-串联质谱，，内标法  Abstract A high performance liquid chromatography-tandem mass spectrometric method was established for simultaneous determination of the nitrofuran metabolites, furazolidone, nitrofurazone and nitrofurantoin in animals，tissue and aquatic produces. Potein-bound metabolites were released in HCl solution and deriatised with 2-nitrobenzaldehyde(2-NBA)overnight at 37℃. Proteins were sedmentated by n-hexane , after adjusting pH to 7.0 by sodium hydroxide. Then the analytes were extracted by ethyl acetate and cleaned up by n-hexane. Identification was achieved by electrospray ionization in positive mode(ESI+) using multiple reaction monitoring(MRM).The quantification was performed with internal standards. The recoveries of 5-methylmorpholino-3-amino-2-oxazolidinone (AMOZ), 3-amino-2-oxazolidimone(AOZ), semicarbazide(SEM) and 1-amino-hydantoin(AHD ) were in the range of 89.5%~110.3%with spiked levels of 0.5~2μg/kg. The RSDs were less than 11.3%. The limits of detection were 0.5μg/kg for AMOZ, AOZ, SEM and AHD. Keywords: Liquid chromatography-tandem mass spectrometric, metabolites of nitrofurans, internal standard.  目 录 摘 要 I Abstract（英文摘要） Ⅱ 目 录 Ⅲ 第一章 引 言 1 1.1硝基呋喃类药物的性质和使用 1.2硝基呋喃类药物的危害及其管理对策 2 1.2.1硝基呋喃类药物的主要危害 2 1.2.2硝基呋喃类药物的管理对策 3 1.3硝基呋喃类物质及其代谢物的样品处理方法 4 1.3.1样品的均质 4 1.3.2提取和衍生化 5 1.3.2.1溶剂提取 5 1.3.2.2水解和衍生化