以超音波輔助分散式液液微萃取結合同步衍生快速檢測水樣中防腐劑成分

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謝智忠(Chih-Chung Hsieh) 查詢紙本館藏

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以超音波輔助分散式液液微萃取結合同步衍生快速檢測水樣中防腐劑成分

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摘要(中)

對羥基苯甲酸酯 (p-hydroxybenzoic acids, Parabens) 作為市面上的防腐劑已經有超過80年的歷史，常添加於沐浴乳、化妝品、藥品及食物中，其價格低廉、無氣味，不易變色、硬化或泥漿化，被世界廣泛接受。但最近研究顯示對羥基苯甲酸酯可能具有雌激素活性、致癌性、造成皮膚病變、刺激眼睛等，為潛在內分泌干擾物。因此，檢測對羥基苯甲酸酯在環境中的濃度是不可避免的趨勢。

本研究開發出一套簡單有效、成本低且快速檢測的方法。使用超音波輔助分散式液液微萃取 (Ultrasonic-assisted dispersive liquid-liquid microextraction, UADLLME) 進行前處理，搭配同步 (in-situ) 衍生化，同時進行萃取及衍生，再利用GC-MS檢測水樣中對羥基苯甲酸酯的含量。

超音波輔助分散式液液微萃取最佳化條件為：將600 μL 異丙醇、300 μL 二氯甲烷和20 μL MTBSTFA+1%TBDMSCl 快速注入含有0.5 g NaCl的 10 ml 水樣中，置於超音波震盪機震盪1 分鐘後，以 4500 rpm 速率離心 10 分鐘，分離有機層及水層，之後放入微波爐中，以 60 瓦的微波功率加熱 150 秒，使衍生更為完全。爾後，取出下層萃取液，進入 GC/MS 進行檢測。在 10-1000 ng/L 的濃度範圍內，檢量線迴歸係數皆大於 0.994；偵測極限 (LOD) 為 0.1-5 ng/L。精密度及準確度測試，其相對標準差 (RSDs) 皆小於 9%，顯示此方法具有良好的穩定性以及再現性。在國內不同水樣中測得的對羥基苯甲酸酯濃度介於 0.045~0.928 μg/L 之間。

摘要(英)

Alkyl p-hydroxybeznoate, also known as Parabens, was added in food, lotion, pharmaceutical and food as preservative for more than 80 years. Because of its odorless, low prices and difficult hardening, they were widely used worldwide. Recent studies show that parabens may contain estrogen, carcinogen activity and potential endocrine disrupter.
A simple, efficient and rapid analysis method for the determination of parabens in aqueous sample is presented. The method involves one-step in-sample silylation coupled with ultrasonic-assisted dispersive liquid-liquid microextraction (UADLLME) prior to their determination by GC-MS.
The optimal extraction condition involved the rapid injection of a mixture of 600μL of 2-propanol (as a dispersant), 300μL of dichloromethane (as an extractant) and 20μL MTBSTFA+1%TBDMSCl (as a derivatizing agent) into a 10 ml of water sample containing 0.5g of sodium chloride in a conical bottom glass tube. After ultrasonication for 1 min and centrifugation at 4500 rpm (10 min), the tube was microwave irradiated at 60W for 150 seconds to accelerate TMS-derivatization.
The limit of quantitations (LOQs) were range between 0.1-5 ng/L. The precision for the analytes, as expressed with relative standard deviation (RSDs), were less than 9%, indicated that this method shows a good stability and reproducibility. In real sample, parabens were detected between 0.04~0.93 μg/L in river samples.

關鍵字(中)

★ 對羥基苯甲酸酯
★ 超音波輔助分散式液液微萃取
★ 同步衍生
★ 氣相層析質譜儀

關鍵字(英)

★ Parabens
★ UADLLME
★ in-situ derivatization
★ GC-MS

論文目次

摘要 I
Abstract III
謝誌 V
目錄 VII
圖目錄 XI
表目錄 XV
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 防腐劑 (Perservative) 5
2-1-1 對-羥基苯甲酸酯簡介 6
2-1-2 分布 8
2-1-3 環境影響 9
2-1-4毒性研究 9
2-1-5 相關檢測文獻 12
2-2 氣相層析質譜儀 19
2-2-1 離子阱質譜儀 21
2-3衍生化介紹 22
2-3-1 矽烷化反應 22
2-4超音波輔助萃取法 24
2-5 分散式液液微萃取法 25
2-5-1 原理 25
2-5-2 分散式液液微萃取法流程 25
2-5-3 影響因素 27
2-5-4 發展 29
2-5-5 超音波輔助分散式液液微萃取 34
2-6 標準添加法 35
2-7 線性迴歸 38
2-7-1 Mandel test 38
2-7-2 The Lack-of-Fit by ANOVA 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 標準品配製 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 水樣採集 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 矽烷基化待測物分析 51
4-1-2 矽烷基化待測物質譜圖 52
4-1-3 檢量線及偵測極限 54
4-2 超音波輔助分散式液液微萃取條件最佳化 55
4-2-1 萃取劑種類 56
4-2-2 分散劑種類 58
4-2-3 萃取劑體積 59
4-2-4 分散劑體積 60
4-2-5 超音波震盪時間 61
4-2-6 鹽類添加量 63
4-2-7 pH值 65
4-2-8 衍生化效率探討 66
4-2-9 超音波輔助分散式液液微萃取最佳化結果 69
4-3 Mandel test & Lack of fit 70
4-3-1 Mandel test 70
4-3-2 Lack of fit 71
4-4 真實樣品檢測 72
4-5 方法精密度與準確度 87
4-6 方法比較 88
第五章結論 91
第六章參考文獻 93
附錄 111

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指導教授

丁望賢(Wang-Hsien Ding)

審核日期

2016-6-20

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