利用深共熔溶劑結合超音波輔助液液微萃取法檢測茶樣中防曬乳成分之殘留

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題名:	利用深共熔溶劑結合超音波輔助液液微萃取法檢測茶樣中防曬乳成分之殘留
作者:	趙惠群;Zhao, Hui-Qun
貢獻者:	化學學系
關鍵詞:	深共熔溶劑;茶樣;Deep eutectic solvent;tea beverages
日期:	2021-07-01
上傳時間:	2021-12-07 11:10:32 (UTC+8)
出版者:	國立中央大學
摘要:	本研究開發一種簡易快速、符合綠色化學的方法檢測茶樣中六種防曬乳成分－二苯基甲酮 b enzophenones 簡稱 BPs) 的殘留。深共熔溶劑為一種新興綠色化學溶劑，具有原料便宜且對環境友善、合成簡單等優點，因此本研究以疏水性深共熔溶劑取代傳統毒性較高的有機溶劑作為萃取劑，選擇氯化膽鹼及對氯苯酚以莫耳比 1 :2 進行合成，並結合超音波輔助液液萃取法 (Deep eutectic solvent based ultrasonic assisted liquid liquid microextraction, 簡稱 DES USALLME) 從茶樣萃取待測物，接著利用超高效液相層析儀串聯電灑游離法四極桿飛行時間質譜儀 U HPLC ESI(+) QTOF MS) 進行測定。實驗數據以多變量實驗設計法中的 M in run screen 及 Central composite design(CCD)中反應曲面法和多變量分析 ( 進行各項因子最佳化。所得最佳條件為：於玻璃離心管中加入 5 mL 茶樣和 70 m g MgSO 4 並 vortex 數秒使鹽類完全溶解，再加入 700 μL DES ，以 vortex 約 10 秒使茶樣和 DES 稍微混合，放入 30 ℃ 的超音波水浴槽震盪 5 分鐘，接著以 3000 rpm 離心 10 分鐘，取出約 440 μL DES 層下層並以甲醇稀釋至 1 m L 。最後將 2 μ L 提取物直接注入 U H PLC QTOF MS 進行檢測分析。所開發方法的定量極限 ( 為 1.8 至 10 ng/mL 。在 i ntra day 及 inter day 的測試中，相對標準偏差 RSD) 皆小於 15 % %，回收率在 74 % 至 127 % 之間，顯示其方法有良好穩定性及再現性。最後以 DES USALLME 結合高選擇性和高靈敏度的 U HPLC ESI(+) QTOF MS 成功應用於真實茶樣的檢測中，包含紅茶、綠茶及烏龍茶，來源分別有茶包、一般手搖店及便利商店中的罐裝茶，其中有檢測出 2OH BP 的微量殘留。;In this study, a simple, efficient, and environmental friendly method for the determination of the presence of six benzophenone type (BPs) UV filters in tea beverages was develops. Due to fulfill the requirements of green analytical chemistry and sustai nable development, a novel “green” solvent, deep eutectic solvent (DES), was replaced traditional halogenated organic solvents using as the extracting solvent. This DES was based on the mixture of choline chloride and 4 chlorophenol at molar ratio of 1:2. The target analytes were effectively extracted from tea beverages using a d eep eutectic solvents based ultrasonic assisted liquid liquid micro extraction (DES USALLME), and their determination were then performed by the combination of ultrahigh performance liquid chromatography and electrospray ionization(+) quadrupole time of f light mass spectrometry (UHPLC ESI(+) QTOF MS). The parameters for the DES USALLME were screened and optimized by multivariate experimental design based on Min run screen and Central composite design (CCD) plus with response surface design and analysis of variance (ANOVA), respectively. The optimal conditions were: a 5 mL of tea beverage mixed with 70 mg of MgSO4 in a glass centrifuge tube.After MgSO4 completely dissolved, a 700 μ L of DES was added and sonicated for 5 min in ultrasonic bath at 30 ℃℃. Then the sample was centrifuged at 3000 rpm for 1 0 min, the DES(about 440 μL) was collected and diluted with methanol to 1 mL. The extract 2 μL was then directly injected into UHPLC QTOF MS for detection. After optimization, the method was validated an d shown to possess low limits of quantification (L OQs) ranged from 1 to 3.2 ng/mL . High precisions and reproducibility (i.e., the relative standard deviations (RSDs) were all less than 15 %) were obtained for both intra and inter day analysis. Satisfact ory average spiked recovery ranged from 74 to 127 %. The developed method was then successfully applied for the analysis of some selected BPs in tea beverages.
顯示於類別:	[化學研究所] 博碩士論文

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