以雙重震盪輔助基質固相分散萃取法檢測室內灰塵中防腐劑parabens成分

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林佳陞(Jia-Sheng Lin) 查詢紙本館藏

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以雙重震盪輔助基質固相分散萃取法檢測室內灰塵中防腐劑parabens成分

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摘要(中)

對-羥基苯甲酸酯 (alkyl p-hydroxybenzoates, 簡稱parabens) 因其價格低廉、無色無味且不易泥漿化及硬化等優點，自20世紀以來被廣泛應用於保養品、化妝品、食物及藥物中。但近年研究指出，parabens具有干擾內分泌系統、雌激素活性，並影響人類生殖系統功能，被列為潛在的內分泌干擾物質。另一方面，人每天皆會暴露在含有室內灰塵的環境中，且室內灰塵為大多數環境汙染物的最終沉澱處，因此有必要開發出一套檢測方法以方便檢測室內灰塵的parabens濃度。
本研究開發出一套快速、有效、同時淨化、且對環境友善的萃取方法來檢測室內灰塵中的 parabens濃度。利用新開發的雙重震盪輔助基質固相分散萃取法 (dual-vortex-assisted matrix solid-phase dispersion, 簡稱DVA-MSPD) 進行樣品前處理，並搭配同位素內標稀釋法 (isotope dilution) 結合超高效液相層析串聯質譜儀 (UHPLC-QTOF-MS) 做定性及定量檢測。
本實驗利用實驗統計設計 (statistical experimental design) 法中的Box-Behnken design (BBD) 及變異數分析 (analysis of variance, ANOVA) 來做DVA-MSPD最佳化的條件探討。萃取的最佳化條件為：將0.1 g 室內灰塵、0.1 g 無水硫酸鈉及0.1 g C18以震盪 1 分鐘的方式進行均質化，接著加入5 mL的ACN：MeOH=1:1 (v/v) 萃取劑進行 30 秒震盪，再以 3000 rpm離心 10 分鐘，取出上層萃取液後，吹氮濃縮至乾並回溶至100 µL，取3 µL進樣至UHPLC-QTOF-MS進行檢測。
此九種parabens的定量極限介於0.9 - 2.8 ng/g；在intra-day及inter-day的測試中，相對標準偏差 (RSD) 皆小於8 %。在室內灰塵樣品中，三種parabens：methyl 4-hydroxybenzoate、ethyl 4-hydroxybenzoate及propyl 4-hydroxybenzoate在大部分樣品中皆被檢測到，濃度介於13.3-339.6 ng/g，少數樣品中則有測到butyl 4-hydroxybenzoate，而isopropyl 4-hydroxybenzoate、isobutyl 4-hydroxybenzoate、benzyl 4-hydroxybenzoate、pentyl 4-hydroxybenzoate、hexyl 4-hydroxybenzoate在檢測的樣品中皆沒有被測到，此結果也與我們常用的parabens種類結果符合。

摘要(英)

Alkyl p-hydroxybenzoates, also called parabens, have been widely added to cosmetics, foods, and pharmaceuticals as preservatives in the 20th century due to their low prices, lack of odor and color, and resistances to hardening. According to recent studies, parabens might interfere with the endocrine system and the human reproductive system, and have been classified as a potential endocrine disrupter. People can be exposed to parabens from indoor dusts, since dusts are the final depositional sites of most environmental pollutants. Given the potential danger of parabens, it is necessary to develop a method to analyze parabens in indoor dust.
This study developed a fast, efficient, one step clean-up and eco-friendly analysis method to determine the concentration of parabens in indoor dust. The method involves a newly developed pretreatment method, dual-vortex assisted matrix solid-phase dispersion (DVA-MSPD) coupled with isotope dilution-UHPLC-QTOF-MS detection.
The parameters of DVA-MSPD were optimized by Box-Behnken design and analysis of variance (ANOVA). The optimal conditions of DVA-MSPD were: weighting 0.1 g indoor dust, 0.1 g sodium sulfate anhydrate, and 0.1 g C18 into a centrifuge tube, homogeneously blended by vortex for 1 minute, add 5 mL of extractant (ACN : MeOH = 1:1 v/v), and extract by vortex for 30 seconds. After vortex, the blend was centrifuged at 3000 rpm for 10 minutes, then the supernatant was collected and dried under nitrogen, and reconstituted with methanol to 100 µL. For analysis, a fraction of the 3 µL solution was injected into the UHPLC-QTOF-MS system for quantitation.
The detection limit were 0.9 - 2.8 ng/g. Intra-day and inter-day precisions (% RSD) for nine analytes were less than 8%. In indoor dust samples, methyl 4-hydroxybenzoate, ethyl 4-hydroxybenzoate and propyl 4-hydroxybenzoate were detected in most samples, the concentration of these three parabens were ranged from 13.3 to 339.6 ng/g. butyl 4-hydroxybenzoate was detected in few sample, and isopropyl 4-hydroxybenzoate, isobutyl 4-hydroxybenzoate, benzyl 4-hydroxybenzoate, pentyl 4-hydroxybenzoate, hexyl 4-hydroxybenzoate were not detected in all the samples.

關鍵字(中)

★ 對-羥基苯甲酸酯
★ 雙重震盪輔助基質固相分散萃取法
★ 超高效液相層析儀

關鍵字(英)

論文目次

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研究源起 1
1-2研究目標 3
第二章文獻回顧 5
2-1防腐劑 (Preservative) 5
2-1-1對-羥基苯甲酸酯簡介 6
2-1-2環境流布 8
2-1-3對環境及人體影響 9
2-1-4毒性研究 10
2-1-5相關規範 13
2-1-6相關檢測文獻 14
2-2超高效液相層析高解析串聯質譜儀 21
2-2-1 Core-shell管柱 23
2-3基質固相分散萃取法 25
2-3-1前言 25
2-3-2原理 26
2-3-3步驟 27
2-3-4影響因素 29
2-4雙重震盪輔助基質固相分散萃取法 31
2-5同位素稀釋定量法 32
第三章實驗步驟與樣品分析 33
3-1實驗藥品與設備 33
3-1-1實驗藥品 33
3-1-2儀器設備 36
3-2實驗步驟 37
3-2-1標準品配製 37
3-2-2超高效液相層析串聯質譜儀參數設定 38
3-2-3質量校正 40
3-2-4空白灰塵的淨化 41
3-2-5雙重震盪輔助基質固相分散萃取法實驗步驟 42
3-3灰塵採集 43
第四章結果與討論 45
4-1 UHPLC-QTOF-MS對待測物的測定 45
4-1-1待測物分析 45
4-1-2待測物之質譜圖 47
4-1-3檢量線及偵測極限 50
4-2雙重震盪輔助基質固相分散萃取法最佳化條件探討 51
4-2-1單因子最佳化探討 51
4-2-2雙重震盪輔助基質固相分散萃取法實驗設計最佳化 58
4-2-3因子間交互作用力之探討 61
4-3 Mandel test & The Lack-of-Fit test 67
4-3-1 Mandel test 67
4-3-2 The Lack-of-Fit test 69
4-4真實灰塵樣品之檢測 71
4-5方法精密度與準確度 75
4-6萃取方法比較 76
第五章結論 79
第六章參考文獻 81
附錄 93

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指導教授

丁望賢

審核日期

2018-6-25

推文