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1、工程硕士学位论文食品中微量乌洛托品的检测方法研究作者姓名陈嘉聪工程领域食品工程校内指导教师张立彦校外指导教师甘文静 所在学院轻工与食品学院论文提交日期201307-03Study on detection methods of trace Urotopine in foodA Dissertation Submitted for the Degree of MasterCandidate：Chen jiacongSupervisor：Associate Prof. Zhang liyanSouth China University of Technology Guangzhou, China分
2、类号：0653 学校代号：10561学 号：2 华南理工大学硕士学位论文食品中微量乌洛托品的检测方法研究作者姓名： 陈嘉聪 申请学位级别：工程硕士 工程领域名称：食品工程校内指导教师姓名、职称：张立彦 副教授 校外指导教师姓名、职称：甘文静、高级工程师论文形式： 产品研发 工程设计 应用研究 工程/项目管理 调研报告研究方向： 食品安全检测论文提交日期： 年 月 日 论文答辩日期： 年 月 日学位授予单位：华南理工大学 学位授予日期: 年 月 日答辩委员会成员：主席： 委员： / 摘 要本课题研究的主要内容是食品中微量乌洛托品的检测方法，主要以不同基质的食品为研究对象，研究乌洛托品的定性分析方
3、法和定量分析方法。针对检测机构和执法部门不同的检测需求提供最适用的检测方法。本文的主要研究工作和成果如下：1、快速筛选的定性分析方法研究通过研究超声萃取法代替常规的直接加热法,改进了乌洛托品定性分析的前处理方法。实验表明，采用超声条件为65，45 KHz，萃取时间为10 min，能够有效的提高乌洛托品分解产物的提取率,从而提高定性分析的灵敏度和准确率.本前处理方法分析方法简单，易操作，适用于现场检测和实验室快速筛选。但是，若想确定乌洛托品的具体含量,仍需要对其进行准确的定量分析。2、快速定量的激光拉曼法研究建立了激光拉曼光谱法测定食品中乌洛托品含量的方法，采用激发波长为785 nm，激发功率为
4、200 mw，扫描时间为20 s,以(894 cm13 cm1）的拉曼特征峰作为定量拉曼峰，标准曲线法确定的线性回归方程为Y=6484.1X + 28。685，相关系数为R2=0。9999，方法的相对标准偏差（RSD）为1.14%4。75%，回收率为90.4%109。7，检出限为0.05 mg/kg。具有样品前处理简单、快速,结果准确、灵敏,具有良好的重现性，系统干扰小，检测时间短，检测成本低，系统小型便携，设备操作相对简便等优点，适用于现场快速检测的要求.3。 高效准确的超高压液相色谱-串联质谱法研究建立了超高压液相色谱串联质谱测定食品中乌洛托品高效准确的分析方法。选用C18固相萃取柱对样品
5、进行净化,在ESI+模式下采用多反应监测(MRM）模式进行检测。目标物在Agilent ZORBAX Eclipse(50 mm2.1 mm，1。7 m）色谱柱上实现了有效分离，在3 min左右完成一个样品的分析,相关系数(R2,n=6）大于0.999，检测结果稳定、灵敏。乌洛托品的线性范围为1。050.0 g/L，检出限为0.5 g/kg （LOD,S/N=3)，方法回收率为86。8%102。7%,相对标准偏差（RSD）为0.364.79%。该方法快速、灵敏，适用于食品中乌洛托品的仲裁检测与确证。关键词：乌洛托品；微量;定性；定量 AbstractThe main content of th
6、is research is the determination methods of trace Urotropine in food。 Mainly by the different food matrix as the research object， the methods of qualitative analysis and quantitative analysis were researched. The most suitable detection methods were given according to the requirements of testing ins
7、titutions and law enforcement agencies. The main research work and results are as follows：1、Study on analysis method of rapid screening of qualitativeThrough the study on the ultrasonic extraction method instead of the conventional direct heating method, the pretreatment method for qualitative analy
8、sis of urotropine was improved。 Experiments showed that, by using ultrasonic conditions of 65 ， 45KHz, extraction time 10min， extraction rate of urotropine could effectively improve the decomposition products and the sensitivity and accuracy. The qualitative analysis method was simple， easy to opera
9、te, suitable for field test and laboratory screening. However， in order to determine the specific content of urotropine, accurate quantitative analysis should be carried out。2、Study on Laser Raman method for rapid quantitativeMethod for the determination of urotropine in food by laser Raman spectros
10、copy was established. The excitation wavelength is 785 nm, the excitation power is 200 MW， and the scanning time of 20 s， with （894cm-1 + 3cm-1) Raman peaks as quantitative Raman peak. the linear regression equation of standard curve method for the determination wasY = 6484。1X + 28。685 the correlati
11、on coefficient is R2=0。9999, and the relative standard deviation was 1。144。75%。 The recovery rate was up to 90。4109.7% and the detection limit is 0。05 mg/kg. The sample pretreatment was simple. This method was rapid， accurate and sensitive, and has good reproducibility and short detection time. The
12、interference of the system is small It was low cost, small and portable and the equipment operation is relatively simple. The method was suitable for on-site rapid detection requirements.3、Study on the accurate and efficient UPLC-MS/MS method UPLC-MS/MS method was established for the efficient and a
13、ccurate determination of urotropine in food。 Purification of the samples were carried out by C18 column， using C18 SPE cartridge and multiple reaction monitoring under the mode of ESI+ （MRM） model to detect. The object in Agilent ZORBAX Eclipse （50 mm 2.1 mm, 1。7 m） column was separated efficiently。
14、 About 3 min was taken to complete a analysis of a sample。 The correlation coefficient （R2, n=6） was greater than 0.999 and the test results were stable， sensitive. The linear range was 1.050.0 g/L of urotropine and the detection limit was 0.5 g/kg (LOD, S/N=3）. the recoveries was 86。8102。7 and prec
15、ision RSD was 0。36 4。79%。 The method was rapid， sensitive and suitable for the detection and confirmation of urotropine in food products. Keywords：Urotopine； Trace； Qualitative； Quantitative目 录摘 要IAbstractII第一章 绪论11。1 乌洛托品对健康的危害11。1。1 乌洛托品简介11.1。2 乌洛托品分解产物甲醛对健康的危害21.1。3 乌洛托品分解产物氨对健康的危害31。2 乌洛托品的作用机理及性质41。3 国内外研究现状51.4 课题研究背景及意义81.5 课题研究的主要内容及方法81。5。1 研究主要
