复杂体系中微量成分的质谱分析方法研究

发布时间：2018-06-27 21:47

本文选题：质谱 + 复杂体系　；参考：《上海师范大学》2017年硕士论文

【摘要】：复杂体系中,尤其是复杂食品体系中的微量成分,正在日益影响着人们的生活。有益的微量成分对于促进人的生长发育、维持新陈代谢、疾病控制及防治等扮演着重要的角色;相反的,有害的微量成分则大多为重要的环境和食品污染物,严重影响着人体健康,进而导致内分泌系统紊乱、癌症等疾病。这些微量成分通常是在食品加工生产时引入,但部分有害微量成分会在食品包装、贮藏、运输等过程中引入;同时,部分食品中有益微量成分的缺失或过量添加也在危害人们的健康。因此,复杂食品体系中微量成分的定性定量检测正在成为食品生产过程及出厂销售前后必不可少的食品安全检测手段,具有十分重要的意义。质谱作为一种具有高灵敏度、高准确性、高效的大型分析仪器,从20世纪20年代开始逐渐成为一种被化学家采用的分析仪器。在众多的分析方法中,质谱法也被认为是一种兼备高灵敏度和高特异性且在食品、药物、材料分析等领域得到广泛应用的仪器分析方法。但由于食品体系的复杂性以及目标物种类的多样性,传统的质谱分析方法在样品前处理、目标物选择性、样品分析速度等方面面临一定的困难。本文系统阐述了质谱法的基本理论及应用,并且针对复杂食品体系,在前人研究的基础上用质谱分析技术作了以下工作:1、结合冷冻前处理和羧基衍生化技术,建立了一种针对奶粉中游离脂肪酸的质谱分析技术。由于高效的冷冻提取法,整个实验流程显示出对对于游离脂肪酸分析效率的显著提高。另外,此实验的优势还在于它的高灵敏度以及大大降低了复杂食品体系的基质效应。在一些国内外奶粉样品中,14种游离脂肪酸被成功检测出来。在不同样品中脂肪酸的含量不尽相同,这可能表明奶粉的质量有所不同。实验成果有望成为复杂基质中游离脂肪酸分析的实用分析方法。2、建立了一种新型混合吸附剂提取净化、气相色谱-串联质谱法测定多种食品包装材料中多环芳烃的方法。新型吸附剂的使用简化了样品的前处理过程,提高了除杂效率同时减少了提取的损失。相比于传统的固相萃取,新型吸附剂的引入缩短了样品前处理的时间;同时,相比与一些经典的吸附剂,新型吸附剂在除杂的种类和效率上有明显提高,有效降低了复杂基底的干扰。同位素内标法提高了定性及定量分析的准确性。方法简便,回收率高,有望用于大批量样品的快速检测。3、在前人研究的基础上,对于低温火焰离子化-敞开式质谱法做了一定的改良,建立了一种基于改良的低温火焰离子化-敞开式质谱法的邻苯二甲酸酯分析方法。敞开式质谱分析大大缩短了样品的分析时间,提高了样品分析效率。低温火焰离子化法保证了样品在进样时的稳定性。该方法成功对7种欧盟及美国相关法律法规规定的邻苯二甲酸酯类物质进行了分析。可为食品及包装材料等中的邻苯二甲酸酯类物质的快速检测提供科学依据。
[Abstract]:The trace components in complex systems, especially in the complex food system, are increasingly affecting people's lives. Beneficial trace elements play an important role in promoting human growth, maintaining metabolism, disease control and prevention and control; and, on the contrary, the harmful micro components are mostly important environmental and food contaminants. It affects human health, which leads to endocrine disorders, cancer and other diseases. These trace elements are usually introduced in food processing, but some harmful trace elements are introduced in the process of food packaging, storage, transportation and other processes; meanwhile, the lack or excessive addition of beneficial trace ingredients in some foods is also harmful to people's health. Therefore, the qualitative and quantitative detection of trace components in the complex food system is becoming a necessary means of food safety inspection before and after the production process of food and the sale of the factory. As a high sensitivity, high accuracy and efficient analysis instrument, mass spectrometry has gradually become a kind of analytical instrument from 1920s. An analytical instrument used by chemists. In many analytical methods, mass spectrometry is also considered to be a highly sensitive and highly specific method of instrumental analysis that has been widely used in food, drug, material analysis and other fields. However, because of the complexity of the food system and the diversity of the species of the target, the traditional mass spectrometry The analysis method is faced with some difficulties in the sample pretreatment, the selectivity of the target, the speed of the sample analysis. This paper systematically expounds the basic theory and application of the mass spectrometry, and makes the following work on the complex food system based on the previous research. 1, combined with the prefreezing pretreatment and carboxyl derivative technology, A mass spectrometric analysis of free fatty acids in milk powder was established. The whole process showed a significant increase in the efficiency of free fatty acid analysis due to high efficiency freeze extraction. The advantage of the experiment was also its high sensitivity and greatly reduced the matrix effect of complex food systems. 14 kinds of free fatty acids have been successfully detected in the samples of external milk powder. The content of fatty acids in different samples is different. This may indicate that the quality of the milk powder is different. The experimental results are expected to be a practical analysis method for the analysis of free fatty acids in the complex matrix.2, and a new type of mixed adsorbent is established to extract and purify the gas chromatograph - The method for the determination of polycyclic aromatic hydrocarbons in various food packaging materials by tandem mass spectrometry. The use of new adsorbents simplifies the pretreatment process of the sample, improves the removal efficiency and reduces the loss of the extraction. Compared with the traditional solid phase extraction, the introduction of new adsorbents shortens the time of sample pretreatment; at the same time, compared with some classics The adsorbents and new adsorbents have obviously improved the types and efficiency of impurity removal and effectively reduce the interference of complex substrates. The isotope internal standard method improves the accuracy of qualitative and quantitative analysis. The method is simple and high recovery rate. It is expected to be used for rapid detection of.3 in large quantities of samples, and on the basis of previous studies, for low temperature flame ionization - A modified low temperature flame ionization - Open mass spectrometric method for the analysis of phthalic acid esters was established by the open mass spectrometry. The analysis time of the sample was greatly shortened by the open mass spectrometry analysis and the efficiency of the sample analysis was improved. The low temperature flame ionization method ensured the stability of the sample in the sample. Methods the phthalic acid esters of 7 kinds of relevant laws and regulations in the EU and the United States were analyzed, and the scientific basis for the rapid detection of phthalic acid esters in food and packaging materials was provided.
【学位授予单位】：上海师范大学
【学位级别】：硕士
【学位授予年份】：2017
【分类号】：TS207.3;O657.63

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