本文選題：游離脂肪酸 + 化學(xué)衍生化��； 參考：《中國農(nóng)業(yè)科學(xué)院》2017年碩士論文

【摘要】：游離脂肪酸(Free fatty acid,FFA)又稱非酯化脂肪酸(nonestesterified fatty acid,NEFA),是類脂代謝物的主要組成部分。在油脂生產(chǎn)和儲(chǔ)存過程中,甘油三酯的水解會(huì)產(chǎn)生FFAs,容易導(dǎo)致油脂的氧化和酸敗,影響油的品質(zhì)和功能。在粗制油中FFAs組成可用于描述壓榨油的質(zhì)量和評(píng)估油損傷程度。FFA成分可以作為油品在不同水分、溫度、含氧量、光照貯藏以及煎炒過程中的降解參數(shù)。食用油中FFA的傳統(tǒng)測定方法是滴定法測定酸價(jià)和氣相色譜法(Gas chromatography,GC)。滴定法測定酸價(jià)得到的是食用油中游離脂肪酸總量,不能對各游離脂肪酸進(jìn)行定性分析,也不能得到各種游離脂肪酸的含量;GC雖然能夠提供食用油中各游離脂肪酸的定性與定量信息,但食用油基質(zhì)復(fù)雜,游離脂肪酸含量低、具有強(qiáng)極性和弱揮發(fā)性,因此需要先經(jīng)過復(fù)雜的樣品前處理以富集和純化游離脂肪酸,然后再將游離脂肪酸進(jìn)行甲酯化衍生后,才能進(jìn)行GC分析,整個(gè)過程非常繁瑣、費(fèi)時(shí),且需要耗費(fèi)大量有機(jī)溶劑,此外,上述方法還存在穩(wěn)定性差,檢測靈敏度低等缺點(diǎn)。因此,建立一種高效、高靈敏度、高通量和高準(zhǔn)確性的分析方法十分有必要。本課題以游離脂肪酸為研究對象,將化學(xué)衍生化技術(shù)與電噴霧串聯(lián)質(zhì)譜(ESI-MS/MS)技術(shù)相結(jié)合,開展基于化學(xué)衍生化技術(shù)的游離脂肪酸高選擇性、高靈敏定性和定量分析新方法研究,以解決現(xiàn)有技術(shù)在游離脂肪酸分析檢測中的技術(shù)瓶頸。本論文研究結(jié)果如下:1.基于衍生化技術(shù)的游離脂肪酸質(zhì)譜分析方法的建立。通過N,N-二乙基乙二胺(DEEA)衍生化技術(shù)結(jié)合鳥槍法-中性丟失掃描-電噴霧質(zhì)譜技術(shù)(shotgun-NLS-ESI-MS/MS),使游離脂肪酸的分析靈敏度提高了2200~6700倍;通過質(zhì)譜中性丟失掃描模式實(shí)現(xiàn)了游離脂肪酸的快速定性分析,結(jié)合內(nèi)標(biāo)進(jìn)行定量分析,為解決游離脂肪酸質(zhì)譜分析離子化效率低,靈敏度差等問題提供了新思路。2.將基于衍生化技術(shù)的質(zhì)譜分析方法應(yīng)用于食用油中游離脂肪酸的定性和定量分析,并將分析結(jié)果和氣相色譜-火焰離子化檢測器(GC-FID)、高效液相色譜-質(zhì)譜聯(lián)用法(HPLC-MS)測得的結(jié)果進(jìn)行了比較,驗(yàn)證了所建立分析方法的可行性。Shotgun-ESI-MS/MS分析方法,樣品前處理簡單,無需經(jīng)過FFAs的分離富集,食用油樣品只需要用正己烷稀釋后便可以進(jìn)行DEEA的衍生化反應(yīng),反應(yīng)完成后即可進(jìn)行質(zhì)譜分析。3.基于衍生化技術(shù)的質(zhì)譜分析方法應(yīng)用于7種食用油中游離脂肪酸的分析。對微波加熱處理不同時(shí)間后的7種食用油中游離脂肪酸組分及含量的變化進(jìn)行了分析,共檢測到食用油中的8種FFAs,其中游離脂肪酸C18:1、C18:2和C18:3經(jīng)微波處理后含量有所增加。4.基于衍生化技術(shù)的質(zhì)譜分析方法應(yīng)用于微波預(yù)處理油菜籽冷榨油中游離脂肪酸的分析。應(yīng)用shotgun-NLS-ESI-MS/MS方法共檢測到菜籽油中8種游離脂肪酸,微波預(yù)處理后的油菜籽冷榨油中游離脂肪酸含量有所增加。結(jié)合主成分分析,成功的區(qū)分了不同來源的冷榨菜籽油。所建立的游離脂肪酸檢測方法簡單有效,能夠有效監(jiān)控菜籽油中游離脂肪酸的含量變化,對保障油品安全與品質(zhì)具有重要的意義。
[Abstract]:Free fatty acid (FFA), also known as non esterified fatty acids (nonestesterified fatty acid, NEFA), is the main component of lipid metabolites. In the process of oil production and storage, the hydrolysis of triglycerides will produce FFAs, which can easily lead to the oxidation and failure of oil and affect the quality and function of oil. The composition of FFAs in crude oil can be made. The.FFA components used to describe the quality of the press oil and the assessment of the degree of oil damage can be used as the degradation parameters in the process of different moisture, temperature, oxygen content, light storage and frying. The traditional method for determination of FFA in edible oil is the titration method for the determination of acid value and gas chromatography (Gas chromatography, GC). The titration method for the determination of acid value is obtained. The total amount of free fatty acids in edible oil can not be qualitatively analyzed and the content of free fatty acids can not be obtained. Although GC can provide qualitative and quantitative information of free fatty acids in edible oil, the base of edible oil is complex, the content of free fatty acid is low, and it has strong and weak volatility. Therefore, it needs first. After complex sample pretreatment, the free fatty acids are enriched and purified, and then the free fatty acids can be methylated and derivatized to carry out GC analysis. The whole process is tedious, time-consuming, and requires a lot of organic solvents. In addition, the methods also have the disadvantages of poor stability and low detection sensitivity. Therefore, a kind of high efficiency is established. The analytical method of high sensitivity, high throughput and high accuracy is very necessary. This subject takes the free fatty acid as the research object, combines the chemical derivatization technology with the electrospray ionization tandem mass spectrometry (ESI-MS/MS) technology to develop the high selectivity of free fatty acids based on chemical derivatization technology, and study the new method of high sensitivity qualitative and quantitative analysis. To solve the technical bottlenecks of free fatty acid analysis and detection of existing technologies. The results of this paper are as follows: 1. based on the establishment of free fatty acid mass spectrometry analysis method based on derivatization technology, N, N- two ethyl ethylenediamine (DEEA) derivatization technology combined with the method of bird shooting neutral loss scanning electrospray mass spectrometry (shotgun-NLS-ESI-MS/MS) The sensitivity of the analysis of fatty acids increased by 2200~6700 times. The rapid qualitative analysis of free fatty acids was realized by the neutral loss scanning mode of mass spectrometry and quantitative analysis combined with the internal standard. A new idea was provided to solve the problems such as low ionization efficiency and poor sensitivity of free fatty acid mass spectrometry analysis..2. will be based on the mass spectrometry based on the derivatization technology. The analytical method was applied to the qualitative and quantitative analysis of free fatty acids in edible oil, and the results were compared with the results obtained by gas chromatography flame ionization detector (GC-FID) and high performance liquid chromatography mass spectrometry (HPLC-MS). The feasibility of the analytical method and the sample pretreatment were verified. Simple, without the separation and enrichment of FFAs, the edible oil samples only need to be diluted with hexane to carry out the derivative reaction of DEEA. After the reaction is completed, the mass spectrometric analysis of.3. is applied to the analysis of free fatty acids in 7 kinds of edible oils. 7 kinds after microwave heating are treated at different time. Analysis of the changes of free fatty acid components and content in edible oil, 8 kinds of FFAs in edible oil were detected. The content of free fatty acid C18:1, C18:2 and C18:3 increased after microwave treatment..4. based on the analysis of mass spectrometry based on derivatization technology was applied to the analysis of free fatty acids in the cold pressing oil of Rapeseed by microwave pretreatment. 8 kinds of free fatty acids in rapeseed oil were detected by shotgun-NLS-ESI-MS/MS method. The content of free fatty acids in the cold pressed oil from rapeseed after microwave pretreatment was increased. The cold pressed rapeseed oil from different sources was successfully distinguished by the combination of principal component analysis. The free fatty acid detection method was simple and effective and can effectively monitor rapeseed oil. The change of free fatty acids in oil plays an important role in ensuring the safety and quality of oil products.
【學(xué)位授予單位】：中國農(nóng)業(yè)科學(xué)院
【學(xué)位級(jí)別】：碩士
【學(xué)位授予年份】：2017
【分類號(hào)】：TQ645.6;O657.63

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