以雙重震盪搭配超音波輔助基質固相分散萃取法快速檢測魚體中 雙酚類內分泌干擾物的殘留

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姓名

林則佑(Ze-You Lin) 查詢紙本館藏

畢業系所

化學學系

論文名稱

以雙重震盪搭配超音波輔助基質固相分散萃取法快速檢測魚體中雙酚類內分泌干擾物的殘留

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摘要(中)

本篇研究中開發了一套快速有效且簡單的方法，來檢測市售魚體中的四種雙酚類內分泌干擾物(BPF、BPE、BPA以及BPB)。本實驗以雙重震盪搭配超音波輔助基質固相分散萃取法(DVUA-MSPD)作為前處理方法，並透過線上醯化氣相層析質譜儀定性及定量。
　　本實驗 DVUA-MSPD的最佳萃取結果由實驗設計 Box-Behnken desigh 搭配反應曲面法得出。最佳化後 DVUA-MSPD的結果是：將0.2 g 的魚粉與1 g 的 PSA 吸附劑加入玻璃離心管中，並透過Vortex 均質化5分鐘。將去離子水 10 mL 加入後以超音波震盪在 30 ℃ 萃取30分鐘，接著加入 10 mL 的乙酸乙酯和1.5克的氯化鈉並震盪10分鐘，接著以2500轉離心10分鐘，取出上清液吹氮至乾。將萃取物以50 μL 二氯甲烷回溶，接著取出4 μL萃取液和2 μL 乙酸酐混合，接著以線上醯化氣相層析質譜儀進樣分析。
　　此方法的定量極限為 0.7 至 4.5 ng/g (乾重)，且在六個濃度下的檢量線皆展現了良好的線性關係(R2大於0.994)。Intra- / Inter-day 的結果回收率介於 71 - 107% 之間，標準差介於 4 – 13% 之間，表示此實驗有良好的精密度與準確度。經最佳化後的DVUA-MSPD前處理搭配線上醯化氣相層析質譜儀，成功快速的檢測魚類中雙酚類內分泌干擾物殘留，且在市售魚體中測得的濃度介於 n.d – 129.2 ng/g (乾重)。

摘要(英)

In this study, an effective and simplified method for the rapid determination of four bisphenolic endocrine-disrupting chemicals (EDCs, bisphenol F, bisphenol E, bisphenol A and bisphenol B) in marketed fish samples was developed. This method employed novel double-vortex- ultrasonic assisted matrix solid-phase dispersion (DVUA-MSPD) technique before identification and quantitation of the target analytes via on-line acetylation gas chromatography-mass spectrometry (GC-MS).
The parameters of DVUA-MSPD extraction were optimized by Box- Behnken design couple with response surface methodology. The optimal conditions of DVUA-MSPD were: a powdered fish sample 0.2 g was dispersed with 1 g of PSA dispersant in a centrifuge tube, and the resulting sample was homogenized by vortex-blending for 5 min. Deionized water (10 mL) was added and the solution was subjected to ultrasonic-extraction in an ultrasonic bath for 30 min at 30 ℃. Ethyl acetate (10 mL) as extractant and 1.5 g of sodium chloride were added to the solution, and the mixture was then vortex for another 10 min. The phases were separated by centrifugation at 2500 rpm for 10 min. The supernatant was collected and evaporated to dryness under a stream of nitrogen. The residue was then re-dissolved in 50 μL of dichloro- methane. Then, the extract 4 μL was mixed with 2 μL of acetic anhydride, and the target analytes were detected subsequently by on-line acetylation GC-MS.
The limits of quantification (LOQs) of the developed method varied from 0.7 to 4.5 ng/g (dry weight). Excellent linearities (coefficient of determination (R2) greater than 0.994) were found for each target analyte in the six-level calibration standard curves. Good precisions were obtained for both intra- and inter-day analysis, and ranged from 4 to 13%. Satisfactory average spiked recovery ranged from 71 to 107%. Optimal DVUA-MSPD procedure coupled with on-line acetylation GC-MS was successfully applied for the rapid determination of selected bisphenolic EDCs in fish samples. The total concentrations were detected ranging from n.d. to 129.2 ng/g (dry weight) in various species of marketed fish.

關鍵字(中)

★ 雙酚類內分泌干擾物
★ 雙重震盪

關鍵字(英)

論文目次

目錄
摘要 i
Abstract iii
謝誌 v
目錄 vii
圖目錄 x
表目錄 xii
第一章前言 1
1-1研究緣起 1
1-2 研究目標 2
第二章文獻回顧 3
2-1 基質固相分散萃取法 3
2-2 雙重震盪搭配超音波輔助基質固相分散萃取法 5
2-3 待測物結構與性質 9
2-4相關檢測文獻 12
2-5 分析儀器 16
2-6 衍生化介紹 19
2-6-1 醯化反應 19
2-6-2 氣相層析質譜儀線上衍生化技術 20
2-7 實驗設計 22
2-8 線性回歸 25
2-9 脂質定量分析 27
第三章實驗步驟與樣品分析 29
3-1 實驗藥品與設備 29
3-2-1 標準品的配置 32
3-2-2氣相層析質譜儀參數設定 33
3-3 DVUA-MSPD 萃取法實驗步驟 35
3-4 空白魚體粉末的淨化 36
3-5 生物檢體採集 36
3-6 脂質定量分析實驗步驟 37
第四章結果與討論 39
4-1 氣相層析儀對乙醯基化待測物的測定 39
4-2 雙重震盪輔助基質固相分散萃取法 43
4-3 檢量線及偵測極限 54
4-4 Mandel test 55
4-5 方法準確度與精密度 56
4-6 真實樣品檢測 57
4-7 前處理方法比較 61
4-8 Analytical Eco-Scale 62
第五章結論 65
第六章參考文獻 67
附錄 73
附錄A F table for α=0.05 73
附錄B 各別待測物ANOVA分析結果及反應曲面圖 74

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指導教授

丁望賢(Wang-Hsien Ding)

審核日期

2020-7-20

推文