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博碩士論文 etd-0624115-131439 詳細資訊
Title page for etd-0624115-131439
論文名稱
Title
熱脫附電噴灑游離質譜法結合多變量分析快速辨識食用油品
Thermal Desorption-Electrospray Ionization/Mass Spectrometry (TD-ESI/MS) Combined with Multivariate Analysis for Rapid Identification of Cooking Oils
系所名稱
Department
畢業學年期
Year, semester
語文別
Language
學位類別
Degree
頁數
Number of pages
84
研究生
Author
指導教授
Advisor
召集委員
Convenor
口試委員
Advisory Committee
口試日期
Date of Exam
2015-07-10
繳交日期
Date of Submission
2015-07-24
關鍵字
Keywords
熱脫附電噴灑游離質譜法、食用油品、三酸甘油酯、多變量分析、油脂、脂肪
Cooking oils, Oils, Thermal Desorption-Electrospray Ionization/Mass Spectrometry, Fats, Multivariate Analysis, Triglycerides
統計
Statistics
本論文已被瀏覽 5650 次,被下載 97
The thesis/dissertation has been browsed 5650 times, has been downloaded 97 times.
中文摘要
近年來,台灣的食用油品問題不斷,使用回收油及油品混摻事件層出不窮,使台灣人民在食品的選購上感到不安並重創台灣在國際間的形象。綜觀回收油與混摻油品,其與正常油品的最大差異在於其可能是由兩種以上食用油品混合而成的,故其與正常油品的三酸甘油酯 (Triglycerides, TG) 組成有所不同。傳統檢測三酸甘油酯的方法是氣相層析-火焰離子化偵測器 (Gas chromatography-flame ionization detector, GC-FID),但繁複的樣品前處理降低了GC-FID的分析速度。比起GC,大氣質譜法 (Ambient mass spectrometry, AMS)只需少量或不需樣品前處理,讓分析變得非常快速且高通量,本研究使用的熱脫附電噴灑游離質譜法 (Thermal desorption-electrospray ionization/mass spectrometry, TD-ESI/MS) 結合多變量分析快速辨識食用油品。
TD-ESI/MS操作非常簡單,只需要用探針輕輕刮取樣品表面,取得微量樣品後,再放入熱脫附裝置中進行分析物的汽化,接著藉由載流氮氣 (Carrier gas)將分析物送至電噴灑游離 (Electrospray ionization, ESI) 區域進行後游離 (Post-ionization) ,離子進入質譜內便可得到訊號圖譜,再搭配多變量分析 (Multivariate analysis),可以達到快速分群,將複雜的圖譜與統計結果以點與點之間距離遠近的方式呈現。
本篇論文分四部份,第一部份是TD-ESI/MS分析食用油品的方法開發,對TD-ESI/MS分析食用油品做最適化探討。第二部分是方法的驗證,以ESI/MS驗證TD-ESI/MS的可行性。第三部份則是以TD-ESI/MS搭配多變量分析來分析食用油品中的三酸甘油酯型態 (TG profiles),已成功的辨識各式食用油品及各種食品 (便當、薯條、洋芋片、沙茶醬、泡麵油包、餅及麵包)的表面的食用油品。在進行混油的區分,可區分4種食用油品 (豬油、大豆油、棕櫚油及橄欖油)不同比例的混摻。第四部分則是監控加熱油品的變化並記錄食用油品的衰敗。
Abstract
Recently, oil mixtures and recycled oils have also been added to cooking oils, deceiving consumers and endangering their health, so that elucidation of oil components is of increasing importance. Oil mixtures and recycled oils have different triglyceride (TG) compositions compared to normal oils. Traditional TG detection methods use gas chromatography-flame ionization detector (GC-FID) after saponification and methyl esterification, which is tedious and time-consuming. Compared to GC, ambient mass spectrometry (AMS) significantly reduces analytical times because it avoids complex sample pretreatment. In this study, an AMS technique known as thermal desorption-electrospray ionization/mass spectrometry (TD-ESI/MS) combined with multivariate analysis was used to rapidly classify various cooking oils.
The ambient TD-ESI source consisted of (1) a sampling probe to obtain analytes from solid or liquid samples, (2) a heated oven for thermally desorbing analytes from the sampling probe, and (3) an ESI source for post-ionizing analytes via interactions with reactive species produced by ESI. The mass spectra obtained from TD-ESI/MS were then analyzed using multivariate analysis software.
This study is divided into four parts. First, we find optimum conditions of cooking oil analysis using TD-ESI/MS. The second is method validation. We verify the correctness of cooking oil analysis using TD-ESI/MS via ESI/MS. Third, we used TD-ESI/MS combined with multivariate analysis to rapidly classify various cooking oils and identify cooking oils in food products such as lunchboxes, fries, potato chips, barbeque sauces, instant noodles, cookies, and bread. TD-ESI/MS was also successfully applied to distinguish components in different oil mixtures (i.e. lard, soybean oil, palm oil, and olive oil). Finally, TD-ESI/MS was used to monitor cooking oil at heating and record the decompose of cooking oil in high temperature.
目次 Table of Contents
論文審定書 i
謝誌 ii
中文摘要 iii
英文摘要 iv
目錄 v
圖目錄 vii
表目錄 xi
第一章、緒論 1
第一節、前言 1
第二節、三酸甘油酯 2
第三節、三酸甘油酯分析方法 4
第四節、現代游離法 5
1. 電噴灑游離法 5
2. 大氣壓力化學游離法15 7
3. 基質輔助雷射脫附游離法17 7
第五節、大氣質譜法(Ambient mass spectrometry)19 8
第六節、大氣質譜法於三酸甘油酯上的應用 11
1. DESI/MS分析三酸甘油酯31 12
2. DART/MS分析三酸甘油酯32 14
3. EASI-MS分析三酸甘油酯 16
第七節、熱脫附電噴灑游離質譜法28 18
第八節、多變量分析 19
第九節、論文目標 20
第二章、實驗 21
第一節、實驗試劑、藥品與真實樣品 21
1. 試劑 21
2. 藥品 21
3. 真實樣品 22
第二節、儀器設備與軟體 24
1. 熱脫附電噴灑游離源28 24
2. 質譜儀 26
3. 主成分分析軟體 26
第三章、結果與討論 27
第一節、開發以熱脫附電噴灑游離質譜法結合多變量分析油品 27
1. 熱脫附電噴灑質譜法針對三酸甘油酯的最適化參數探討 27
2. 取樣方法開發 29
3. 多變量分析參數最適化 34
4. 質譜儀解析度的影響 35
第二節、以電噴灑游離質譜法作方法驗證 36
第三節、以熱脫附電噴灑游離質譜法結合多變量分析辨識油品 40
1. 純油品之辨識及資料庫的建立 40
2. 分析便當使用的油品分析 48
3. 其他食品之油品分析 52
4. 分析混油 58
第四節、以熱脫附電噴灑游離質譜法監控加熱油品的變化 62
第四章、結論 65
第五章、參考文獻 66
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