文档介绍：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
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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***、呋喃它***、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,,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。~2μg/kg范围内,%~%;相对标准偏差(RSD)%。5-马啉代***-3-氨基-2-恶唑***(5-methylmorpholino-3-amino-2-oxazolidinone,AMOZ)、3-氨基-2-恶唑***(3-amino-2-oxazolidinone,AOZ)、氨基脲(semicarbazide,SEM)和1-氨基-乙内酰***(1-amino-hydantoin,AHD)。
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-nitrobenzaldehyde(2-NBA)overnight at 37℃. Proteins were sedmentated by n-hexane , after adjusting pH to 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 %~%with spiked levels of ~2μg/kg. The RSDs were less than %. The limits of detection were for AMOZ, AOZ, SEM and AHD.
Keywords: Liquid chromatography-tandem mass spectrometric, metabolites of nitrofurans, internal standard.
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摘要 I
ABSTRACT(英文摘要) Ⅱ
目录Ⅲ
第一章引言 1
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(LLP) 6
(MSPD) 6
(SPE) 7