以基質固相分散萃取法搭配線上衍生氣相層析串聯式質譜儀檢測環境生物檢體中防曬乳成份含量

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蔡東穎(Dung-Ying Tsai) 查詢紙本館藏

畢業系所

化學學系

論文名稱

以基質固相分散萃取法搭配線上衍生氣相層析串聯式質譜儀檢測環境生物檢體中防曬乳成份含量

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摘要(中)

有機防曬乳成份(organic UV filters)是一種廣泛添加於防曬乳、化妝品以及保養品等各種產品中的化合物，在生產及使用過程中，易由水途徑進入環境中。近年來研究指出脂溶性較高的有機防曬乳成份會累積於魚體中，經由食物鏈累積於人體內，可能會造成內分泌干擾，而危害人體健康，近年來已被歸類為新興汙染物(Emerging contaminants，ECs)的一種。
本研究是利用基質固相分散萃取法(Matrix solid¬¬¬ phase dispersion extraction，MSPD)來檢測生物檢體中的有機防曬乳成份，並利用實驗統計設計(statistical experimental design)及變異數分析(analysis of variance，ANOVA)來做最佳化的探討。最佳化後的基質固相分散萃取條件為:以0.5 g生物檢體與1 g矽酸鎂均勻混合，填入含有1 g C18的固相萃取夾中，再用7 ml乙腈沖堤出來，並以氮氣吹乾後用內標準品回溶。取10 μL待測物溶液利用大體積樣品導入裝置進行線上(on-line)矽烷化衍生，搭配氣相層析串聯式質譜儀(Gas Chromatography- Tandem mass spectrometry, GC-MS/MS)來偵測，可得偵測極限皆小於0.1 ng/g。在生物檢體中，防曬乳成份的總濃度介於0.5至51.2 ng/g。

摘要(英)

Organic UV filters are a group of chemicals used widely in sunscreen, cosmetic and skin care products to protect skin from damaging UV radiation. After use, organic UV filters are washed off from skin and clothes, and enter the aquatic environment. Recent studies indicate that some lipophilic UV filters can be accumulated in biota and act as endocrine disruptors. Organic UV filters are considered as one kind of the emerging pollutants in the environment.
In this study, a rapid procedure, Matrix solid-phase dispersion (MSPD), was developed to extract five commonly used organic UV filters: EHS, HMS, BP-3, BP-1 and BP-8, from biota samples. The parameters affecting the MSPD extraction efficiency was systematically investigated by statistical experimental design and analysis of variance. For optimal conditions of MSPD are：0.5 g of fish sample dispersing with 1 g Florisil was packed into the SPE column which contains 1.0 g of octadecyl bonded silica (C18), as the clean-up co-sorbent. The target analytes were then eluted with 7 mL of acetonitrile. The extract was adjusted to 100 L, and on-line derivatized in the GC injection-port with a trimethylsilylated (TMS) reagent. The TMS-derivatives were then identified and quantitated by gas chromatography-tandem mass spectrometry (GCMS/MS). The limits of detection (LODs) were less than 0.1 ng/g. The total concentrations of these organic UV filter residues in biota samples ranged from 0.5 to 51.2 ng/g.

關鍵字(中)

★ 氣相層析
★ 基質固相分散萃取法

關鍵字(英)

論文目次

中文摘要 I
英文摘要 II
謝誌 IV
圖目錄 IX
表目錄 XI
第一章前言 1
1-1 研究緣起 1
1-2 研究目標 3
第二章文獻回顧 5
2-1 新興汙染物 (Emerging contaminants) 5
2-2 防曬乳成分 7
2-2-1防曬乳成份簡介 7
2-2-2 防曬乳成份的毒性 9
2-2-3 防曬乳成份的性質 11
2-2-4 環境中防曬乳成分的來源 14
2-2-5 國外相關文獻 16
2-3 氣相層析質譜儀 18
2-3-1 大體積直接進樣裝置 20
2-3-2 離子阱質譜儀 22
2-4 衍生化技術 23
2-4-1 衍生化技術的種類及條件 23
2-4-2 矽烷化反應 24
2-4-3 線上衍生化技術 25
2-5基質固相分散萃取法 27
2-6 實驗設計 30
2-6-1 實驗設計簡介 30
2-6-2 反應曲面法(Response surface methodology, RSM) 31
2-6-3 Box-Behnken設計 34
2-7 線性迴歸 36
2-8 基質效應 40
第三章實驗步驟與樣品分析 43
3-1 實驗藥品與設備 43
3-1-1 實驗藥品 43
3-1-2 儀器設備 45
3-2 實驗步驟 46
3-2-1 標準品的配置 46
3-2-2 氣相層析質譜儀的參數設定 47
3-2-3 實驗流程 49
3-3 生物檢體採集 50
第四章結果與討論 51
4-1 氣相層析質譜儀對矽烷基化待測物的測定 51
4-1-1 矽烷基化待測物的分析 51
4-1-2 矽烷基化待測物質譜圖 52
4-1-3 串聯式質譜儀 55
4-1-4檢量線及偵測極限 59
4-2 基質固相分散萃取法最佳化條件探討 61
4-2-1 分散吸附劑與沖堤溶劑種類選擇 61
4-2-2 統計實驗設計做MSPD最佳化 63
4-2-3 因子間交互作用力的探討 67
4-3　Mandel test 與 Matrix effect 71
4-3-1　Mandel test 71
4-3-2　The Lack-of-fit test 72
4-3-3　Matrix effect 73
4-4　真實樣品之檢測 75
4-4-1　市售樣品的檢測 75
4-4-2　環境樣品的檢測 80
第五章結論 89
第六章參考文獻 91

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指導教授

丁望賢(Wang-Hsien Ding)

審核日期

2013-7-4

推文