食用油縮水甘油酯組成分析之方法開發

TMUIR > College of Nutrition > Master Program in Food Safety > Dissertations/Theses > Item 987654321/58640

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Title:	食用油縮水甘油酯組成分析之方法開發 Method Development for Determination of Glycidyl Ester Species in Edible Oils
Authors:	吳品儀 Wu, Ping-Yi
Contributors:	食品安全碩士學位學程李偉如
Keywords:	縮水甘油酯;縮水甘油醇;致癌物;食用油;精煉;UPLC-ELSD glycidyl esters;glycidol;carcinogen;edible oil;refine;UPLC-ELSD
Date:	2018-06-30
Issue Date:	2020-02-11 12:49:55 (UTC+8)
Abstract:	油脂精煉過程中的脫臭步驟，因高溫導致油脂裂解重排產生縮水甘油酯(glycidyl esters, GEs)，於體內消化水解形成2A致癌物縮水甘油。本研究之目的為建立檢測精煉食用油中GEs含量之替代方法，利用超高效液相層析法搭配蒸發光散射檢測器開發直接法定量植物油中主要的五種GEs。首先，GEs標準品使用基質輔助雷射脫附飛行時間串聯質譜儀進行定性分析，確認其荷質比與待測物一致。UPLC-ELSD結果顯示BEH C18管柱搭配梯度流洗可以成功分離五種GEs，移動相A、B分別為85%和2.5%甲醇水溶液，流速0.25 mL/min，分析時間25分鐘，注射量為10 µL。ELSD檢測器設定為霧化溫度30°C，蒸發管溫度55°C，氦氣壓力50 psi。將混合標準品的濃度與波峰面積進行迴歸分析，所得到之一次與二次檢量線，皆具有良好的線性，且二次曲線代入結果較一次好(R2>0.99)，以80、50、40 µg/mL濃度GE標準品在同日間與不同日間分析，回收率均在70-120%之間，變異係數均低於10%，顯示具有良好的準確度與精密度。GEs混合標準品於油脂樣品中的添加回收率均在70~120％之間。ELSD檢測五種GEs的定量極限皆為10 µg/mL，方法的定量極限為1.25 µg/mL。以上結果顯示UPLC-ELSD具有潛力開發作為一新穎簡便之替代方法評估精煉油脂中的GEs含量對照歐盟標準。 During the deodorization step in oil refining process, glycidyl esters (GEs) are formed from oil degradation under high-temperature. GEs will further be digested and hydrolyzed to glycidol, which has been classified as Group 2A carcinogen. The aim of this study is to develop an alternative method in order to determine the GEs contents. In this study, 5 main GEs in vegetable oils were quantified using ultra performance liquid chromatography (UPLC) equipped with evaporative light scattering detector (ELSD). First, 5 GE standards were qualified by matrix-assisted laser desorption ionization-time of flight-tandem mass (MALDI-TOF-MS/MS) to confirm the mass to charge ratio (m/z) conforming to targeted analytes. Separation of 5 GE standards was achieved by BEH C18 column combined with gradient elution composed of mobile phase A (85% MeOH) and B (2.5% MeOH). The flow rate was 0.25 mL/min and run time 25 min. The injection volume was 10 µL. ELSD detector conditions were set as nebulizer temperature at 30ºC, drift tube at 55ºC, and nebulizer gas of 50 psi. Regression analysis between concentration and peak area of the GEs showed that the linear and linear-quadratic curves both had good linearity. The coefficient of determination (R2) of linear-quadratic curve was better than linear curve, R2 > 0.99. The intraday and interday recovery (%) of 80, 50 and 40 μg/mL GEs were in the range of 70-120%, and the intraday and interday coefficients of variation (CV%) were below 10%, demonstrating good accuracy and precision. The recovery (%) of GE standards spiked in oil samples were between 70-121%. The limit of quantitation (LOQ) of GE by ELSD was 10 μg/mL, and the LOQ of this method was 1.25 μg/mL. These results indicated that the UPLC-ELSD method has the potential to become a novel and simple alternative method for evaluating GE content in oil against EU regulation.
Description:	碩士指導教授：李偉如委員：蘇南維委員：林士祥
Data Type:	thesis
Appears in Collections:	[Master Program in Food Safety] Dissertations/Theses

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