Please use this identifier to cite or link to this item:
http://tdr.lib.ntu.edu.tw/jspui/handle/123456789/73879
Title: | 開發食用油脂中3-單氯丙二醇酯及縮水甘油酯檢測方法之研究 Studies on Method Development for the Determination of 3-Chloro-1,2-propanediol (MCPD) Fatty Acid Esters and Glycidyl Fatty Acid Esters in Edible Oils |
Authors: | Hsin-Ya Tsai 蔡欣亞 |
Advisor: | 蘇南維(Nan-Wei Su) |
Keyword: | 3-單氯丙二醇酯,縮水甘油酯,改良式QuEChERS,食用油脂,熱加工汙染物, 3-chloro-1,2-propanediol fatty acid esters,glycidyl fatty acid esters,modified QuEChERS,edible oil,heat-induced processing contaminant, |
Publication Year : | 2019 |
Degree: | 碩士 |
Abstract: | 3-單氯丙二醇酯(3-chloro-1,2-propanediol fatty acid esters, 3-MCPDEs)和縮水甘油酯(glycidyl fatty acid esters, GEs)為近年在精煉油脂中發現的熱加工汙染物,由於其對人體健康潛在的疑慮,歐盟執行委員會於2018年訂定食用油脂及嬰兒配方奶粉中GEs之限量(EC No 1881/2006),然而,目前的公定分析方法卻有樣品前處理過於耗時和前處理過程中3-MCPD和 glycidol相互轉換的問題。因此,本研究針對上述問題進行改善,建立一套檢測食用油脂中3-MCPDEs及GEs之分析方法。本研究以酵素水解搭配直接分析glycidol的模式,改善以往方法中酸或鹼水解導致分析物間轉換,以及glycidol鹵素化不完全導致低估等問題。此方法透過酵素水解,藉由脂解酶(lipase)在較溫和的反應條件下(室溫反應30 min)將3-MCPDEs及GEs水解成3-MCPD及glycidol,續利用改良式QuEChERS樣品前處理,加入調整後之萃取用粉劑(6 g無水硫酸鎂和3 g甲酸鈉)及10 mL ACN有效將酵素反應液中高極性的3-MCPD及glycidol萃取至有機層,取一部分檢液直接以GC-MS定量分析glycidol (GEs含量),另取一部分檢液衍生化後利用GC-MS定量分析3-MCPD衍生物(3-MCPDEs含量)。方法確效結果顯示,Glycidol和3-MCPD於檢量線濃度範圍內線性關係良好(R2 ≥ 0.999);定量極限定為0.1 (glycidol) 和0.1 (3-MCPD) μg/g;同日間(intraday)分析之回收率和CV符合食品化學檢驗方法之確效規範。另一部分研究則藉由加熱三酸甘油酯添加不同比例雙酸甘油酯之模式系統,及分別加熱市售豬油和去除極性物質之豬油三酸甘油酯,評估油脂中可能影響GEs生成之因子,結果顯示,市售豬油相對於模式系統油脂於170℃加熱1 h條件下,GEs含量即有顯著增加之趨勢,顯示豬油中極性物質可能有促進GEs生成之效應。 3-Chloro-1,2-propanediol fatty acid esters (3-MCPDEs) and glycidyl fatty acid esters (GEs) are heat-induced processing contaminants in refined edible oils. Due to the potential risk of 3-MCPDEs and GEs to humans, Commission Regulation (EC) No. 1881/2006 have set maximum levels for GEs in foodstuffs in 2018. However, current analytical methods for 3-MCPDEs and GEs are either time consuming or unreliable because of some undesirable side reactions occurring in sample preparation process. Therefore, the objective of this study is to develop a simple and reliable analytical method for 3-MCPDEs and GEs in edible oils. In this work, a method based on lipase hydrolysis and direct determination of free form GEs, glycidol, was successfully achieved by modified QuEChERS. Highly polar glycidol and 3-MCPD were extracted by 10 mL acetonitrile with 6 g magnesium sulfate and 3 g sodium formate from lipase reaction buffer into organic layer for subsequent derivatization (only for 3-MCPD) and GC-MS analysis instead of conversion of glycidol into halogenated PBA derivatives by alkaline/acidic hydrolysis and halogenation in previous analytical approaches, thus avoiding occurrence of unintended side reactions from alkaline/acidic hydrolysis or halogenation steps in sample preparation process. Recovery of each step was evaluated and method validation was further performed to evaluate linearity, limit of quantification (LOQ), accuracy and precision of our developed method. Linearity was verified for both analytes, glycidol and 3-MCPD derivatives (R2 ≥ 0.999). LOQ was set to be 0.1 and 0.1 μg/g on the basis of S/N ratio ≥ 10 for glycidol and 3-MCPD, respectively. Recoveries and CV of intraday analysis met the current method validation guidelines set by Taiwan FDA. Model oil (triacylglycerols separated from soybean oil) spiked with different amount of DAGs, commercial lard and triacylglycerols separated from lard (lard TAGs) were heated at different temperatures to investigate the formation of GEs during heat processing. Results showed that polar compounds in lard may increase GEs formation. |
URI: | http://tdr.lib.ntu.edu.tw/jspui/handle/123456789/73879 |
DOI: | 10.6342/NTU201903644 |
Fulltext Rights: | 有償授權 |
Appears in Collections: | 農業化學系 |
Files in This Item:
File | Size | Format | |
---|---|---|---|
ntu-108-1.pdf Restricted Access | 3.9 MB | Adobe PDF |
Items in DSpace are protected by copyright, with all rights reserved, unless otherwise indicated.