本文選題：質譜 + 復雜體系　； 參考：《上海師范大學》2017年碩士論文

【摘要】：復雜體系中,尤其是復雜食品體系中的微量成分,正在日益影響著人們的生活。有益的微量成分對于促進人的生長發(fā)育、維持新陳代謝、疾病控制及防治等扮演著重要的角色;相反的,有害的微量成分則大多為重要的環(huán)境和食品污染物,嚴重影響著人體健康,進而導致內分泌系統(tǒng)紊亂、癌癥等疾病。這些微量成分通常是在食品加工生產時引入,但部分有害微量成分會在食品包裝、貯藏、運輸等過程中引入;同時,部分食品中有益微量成分的缺失或過量添加也在危害人們的健康。因此,復雜食品體系中微量成分的定性定量檢測正在成為食品生產過程及出廠銷售前后必不可少的食品安全檢測手段,具有十分重要的意義。質譜作為一種具有高靈敏度、高準確性、高效的大型分析儀器,從20世紀20年代開始逐漸成為一種被化學家采用的分析儀器。在眾多的分析方法中,質譜法也被認為是一種兼?zhèn)涓哽`敏度和高特異性且在食品、藥物、材料分析等領域得到廣泛應用的儀器分析方法。但由于食品體系的復雜性以及目標物種類的多樣性,傳統(tǒng)的質譜分析方法在樣品前處理、目標物選擇性、樣品分析速度等方面面臨一定的困難。本文系統(tǒng)闡述了質譜法的基本理論及應用,并且針對復雜食品體系,在前人研究的基礎上用質譜分析技術作了以下工作:1、結合冷凍前處理和羧基衍生化技術,建立了一種針對奶粉中游離脂肪酸的質譜分析技術。由于高效的冷凍提取法,整個實驗流程顯示出對對于游離脂肪酸分析效率的顯著提高。另外,此實驗的優(yōu)勢還在于它的高靈敏度以及大大降低了復雜食品體系的基質效應。在一些國內外奶粉樣品中,14種游離脂肪酸被成功檢測出來。在不同樣品中脂肪酸的含量不盡相同,這可能表明奶粉的質量有所不同。實驗成果有望成為復雜基質中游離脂肪酸分析的實用分析方法。2、建立了一種新型混合吸附劑提取凈化、氣相色譜-串聯質譜法測定多種食品包裝材料中多環(huán)芳烴的方法。新型吸附劑的使用簡化了樣品的前處理過程,提高了除雜效率同時減少了提取的損失。相比于傳統(tǒng)的固相萃取,新型吸附劑的引入縮短了樣品前處理的時間;同時,相比與一些經典的吸附劑,新型吸附劑在除雜的種類和效率上有明顯提高,有效降低了復雜基底的干擾。同位素內標法提高了定性及定量分析的準確性。方法簡便,回收率高,有望用于大批量樣品的快速檢測。3、在前人研究的基礎上,對于低溫火焰離子化-敞開式質譜法做了一定的改良,建立了一種基于改良的低溫火焰離子化-敞開式質譜法的鄰苯二甲酸酯分析方法。敞開式質譜分析大大縮短了樣品的分析時間,提高了樣品分析效率。低溫火焰離子化法保證了樣品在進樣時的穩(wěn)定性。該方法成功對7種歐盟及美國相關法律法規(guī)規(guī)定的鄰苯二甲酸酯類物質進行了分析�？蔀槭称芳鞍b材料等中的鄰苯二甲酸酯類物質的快速檢測提供科學依據。
[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.
【學位授予單位】：上海師范大學
【學位級別】：碩士
【學位授予年份】：2017
【分類號】：TS207.3;O657.63

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