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研究生:楊鈞全
研究生(外文):Chun-Chuan Yang
論文名稱:以基質固相分散萃取法快速檢測水產樣品中溴化阻燃劑
指導教授:丁望賢丁望賢引用關係
指導教授(外文):Wang-Hsien Ding
學位類別:碩士
校院名稱:國立中央大學
系所名稱:化學學系
學門:自然科學學門
學類:化學學類
論文種類:學術論文
論文出版年:2014
畢業學年度:103
語文別:中文
論文頁數:129
中文關鍵詞:溴化阻燃劑基質固相分散萃取法電子捕捉負離子化學游離法生物檢體
外文關鍵詞:brominated flame retardantsmatrix solid-phase dispersionelectron-capture negative ionbiota sample
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溴化阻燃劑如:十溴二苯醚 (Decabromodiphenyl ether, decaBDE)、六溴環十二烷 (Hxabromocyclododecane, HBCD),已是市面上被常用來添加於防火材料中,主要是此兩種化合物在防火部分相較於其他鹵素,僅需少量添加,便可有良好的阻燃效果。這類溴化阻燃劑因具有持久性與高親脂性 (log Kow>5),因此在食物鏈中會累積放大。目前在許多人類常食用的水產中已檢測出含有此類物質。
本研究主要開發一套簡單、有效且可快速檢測這兩種溴化阻燃劑的樣品前處理方法,應用在不同種類生物樣品中。實驗的萃取方法是使用基質固相分散萃取法 (Matrix solid-phase dispersion, MSPD) 來進行樣品前處理,並利用氣相層析質譜儀結合電子捕捉負離子化學游離法 (GC-ECNI-MS) 進行偵測。最佳化的萃取條件為將1 g經由冷凍乾燥的生物樣品和2 g的SiO2,放入震盪器中快速均勻混合。把混合物轉移到含有1 g 30 % 酸性SiO2與1.5 g SiO2的玻璃管柱中,並以20 mL Hexane: DCM=1: 1的比例進行沖提,之後再將萃取液轉移至與上面相同淨化粉末的管柱中,再以10 mL 相同比例進行沖提,最後將萃取液旋濃乾燥。回溶後取1 μL利用GC-ECNI-MS進行檢測分析。
本研究結果顯示萃取回收率在81-108 %之間,其相對標準偏差 (RSDs) 皆小於10 %,顯示此方法具有良好的再現性與穩定性。而decaBDE與HBCD的偵測極限 (LOD) 分別為0.05 ng/g與0.03 ng/g;在真實樣品部分,市售的水產中分別可檢測出decaBDE: 0.34-2.11 ng/g與HBCD: 0.17-0.5 ng/g。
Brominated flame retardants, such as decabromodiphenyl ether (decaBDE),and hxabromocyclododecane (HBCD), are used to add in the fire protection materials. Comparing to other halogen fire section, they have good flame retardant effect by adding only small amount. Because brominated flame retardants are persistent and highly lipophilic (log Kow> 5), they can be bio-accumulated and bio-magnificated in the food chain. Currently in many human regular consumption of biota products have detected containing such substances.
This study was to develop a simple, effective and rapid sample pretreatment of two brominated flame retardants and apply to different types of biological samples. Experimental extraction method involves the use of vortex-homogenization matrix solid-phase dispersion (VHMSPD) extraction for sample pretreatment, and determination by gas chromatography- electron capture negative ion mass spectrometry (GC-ECNI-MS). The optimal extraction conditions involved dispersing of freeze-dried biota sample (1 g) with 2 g of SiO2 by a vigorous shaking to obtain a homogenous mixture. The mixture was transferred to a glass column containing 1 g 30% acidic SiO2 and 1.5 g SiO2 as the clean-up co-sorbent.The target analytes were then eluted with 20 mL of Hexane: DCM = 1: 1.The extract was transferred to the same column described above, and eluted with 10 mL of the same solvent. The extract was adjusted to 1 μL and then determined by GC-ECNI-MS.
The findings show that the extraction recovery was obtained about 81-108% and relative standard deviations (RSDs) are less than 10 %, respectively. It indicats that the method shows good reproducibility and stability. The detection limit of decaBDE and HBCD were 0.05 ng / g and 0.03 ng / g respectively. In real sample section, decaBDE can be detected between 0.34-2.11 ng / g and HBCD can be dected detween 0.17- 0.5 ng / g in marketed sea food samples.
摘要 I
Abstract III
謝誌 V
目錄 VII
圖目錄 XI
表目錄 XIII
第一章 前言 1
1-1 研究緣起 1
1-2 研究目標 4
第二章 文獻回顧 5
2-1 阻燃劑 5
2-1-1 阻燃劑簡介與原理 5
2-1-2 阻燃劑之分類 7
2-1-3 溴化阻燃劑簡介 10
2-2 多溴二苯醚 13
2-2-1 多溴二苯醚簡介 13
2-2-2 多溴二苯醚之性質 15
2-2-3 多溴二苯醚之毒性 17
2-3 六溴環十二烷 19
2-3-1 六溴環十二烷簡介 19
2-3-2 六溴環十二烷之性質 21
2-3-3 六溴環十二烷之毒性 23
2-4 十溴二苯醚與六溴環十二烷檢測之相關研究 24
2-5 基質固相分散萃取法 31
2-5-1 基質固相分散萃取法簡介 31
2-5-2 基質固相分散萃取法原理 32
2-6 氣相層析質譜儀 34
2-6-1 氣相層析質譜儀簡介 34
2-6-2 電子捕捉負離子化學游離法 36
2-6-3 四極矩質譜儀 38
2-6-4 選擇離子偵測法 40
2-7 線性回歸 41
2-7-1 Mandel test 41
2-7-2 The Lack-of-Fit Test 43
2-8 基質效應 45
第三章 實驗步驟與樣品分析 49
3-1 實驗藥品與設備 49
3-1-1 實驗藥品 49
3-1-2 儀器設備 51
3-2 實驗步驟 52
3-2-1 標準品的製備 52
3-2-2 氣相層析質譜儀參數設定 53
3-2-3 基質固相分散萃取法萃取步驟 55
3-2-4 生物檢體採集 56
第四章 結果與討論 57
4-1 溴化阻燃劑 57
4-1-1 氣相層析質譜儀對溴化阻燃劑的檢測 57
4-1-2 檢量線及偵測極限 60
4-2 基質固相分散萃取法最佳化條件探討 62
4-2-1 分散劑種類選擇 62
4-2-2 酸性矽膠濃度的選擇 63
4-2-3 吸附劑探討 64
4-2-4 萃取溶劑探討 65
4-2-5 分散劑體積探討 66
4-2-6 酸性矽膠體積探討 67
4-2-7 吸附劑體積探討 68
4-2-8 萃取溶劑體積探討 69
4-2-9 基質固相分散萃取的最佳化結果 70
4-3 Mandel test 與 The Lack of fit test 71
4-3-1 Mandel test 71
4-3-2 The Lack-of-fit test 72
4-4 基質效應 73
4-5 真實樣品之檢測 75
4-6 檢測方法的穩定性 83
4-7 方法比較 84
第五章 結論 87
第六章 參考文獻 89
附錄 104

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