动物组织中基呋喃代谢物残留量的测定方法.docVIP

动物组织中硝基呋喃代谢物残留量的测定方法 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,?标法定量。在添加浓度0.5~2μg/kg范围内,?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,硝基呋喃类代谢物,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-nitrobenzaldehyde2-NBAovernight 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 modeESI+ using multiple reaction monitoringMRM.The quantification was performed with internal standards. The recoveries of 5-methylmorpholino-3-amino-2-oxazolidinone AMOZ, 3-amino-2-oxazolidimoneAOZ, semicarbazideSEM and 1-amino-hydantoinAHD 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IAbstract(英文摘要) Ⅱ 目 录Ⅲ第一章 引 言11.1硝基呋喃类药物的性质和使用11.2硝基呋喃类药物的危害及其管理对策21.2.1硝基呋喃类药物的主要危害21.2.2硝基呋喃类药物的管理对策31.3硝基呋喃类物质及其代谢物的样品处理方法41.3.1样品的均质41.3.2提取和衍生化51.3.2.1溶剂提取51.3.2.2水解和衍生化51.3.3样品的净化61.3.3.1液液萃取(LLP)61.3.3.2基体固相分散技术(MSPD)61.3.3.3固相萃取技