Please use this identifier to cite or link to this item: http://hdl.handle.net/11455/90617
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dc.contributorJen-Fon Jenen_US
dc.contributor鄭政峰zh_TW
dc.contributor.author李心儀zh_TW
dc.contributor.authorHsin-Yi Lien_US
dc.contributor.other化學系所zh_TW
dc.date2014zh_TW
dc.date.accessioned2015-12-10T02:48:01Z-
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P.; Lores, M.; Garcia-Jares, C.; Llompart, M., Simultaneous in-cell derivatization pressurized liquid extraction for the determination of multiclass preservatives in leave-on cosmetics. Analytical chemistry 2010, 82 (22), 9384-9392.zh_TW
dc.identifier.urihttp://hdl.handle.net/11455/90617-
dc.description.abstractA green analytical method for the determination of parabens in shampoo by pseudo-solvent based cloud point microextraction (PS-CPME) was investigated. In this study, fatty acid was investigated as pseudo-solvent due to it is soluble in basic medium and insoluble (as extractant) in acid medium. After a dilution of shampoo sample with water, parabens in 5 mL aqueous sample solution were measured under the selected conditions. A home-made glass extraction barrel inbuilt with a scaled capillary tube was utilized as a PS-CPME device to collect the separated extractant. 40μL of heptanoic acid (as pseudo-solvent) and 30μL of NH4OH were added into a 8 mL extraction barrel filled with 5 mL sample solution, after shakily mixing for 10 sec, 750 mg of NaCl and 600μL of H2SO4 was added and also shake for 10 sec to form the insoluble heptanoic acid. The cloudy solution was centrifuged at 3200 rpm for 1min, and the separated extractant was push into scaled capillary tube and collected 10μL for HPLC analysis. Under these conditions, the linear dynamic range for the detection was 0.04-8μg/mL for methyl paraben, 0.02-4 μg/mL for ethyl paraben, and 0.01-2 μg/mL for propyl paraben and butyl paraben, with relative standard derivation (RSD) below 6.8%. Detection limits were achieved at the level of 0.0005-0.008 μg/mL. Quantitative limits were achieved at the level of 0.002-0.03 μg/mL. Recoveries were ranged in between 92.2% to 104.1% and its RSD less than 8.8%. The proposed PS-CPME method was proven to be a simple, rapid, low-cost and eco-friendly sample preparation process to extract parabens in shampoo samples for chromatographic analysis.en_US
dc.description.abstract本研究利用有機酸所具有之溶劑與界面活性劑轉換特性開發為雲點 萃取之前處理技術,結合高效能液相層析儀 (HPLC-UV),檢測洗髮精中 四種對羥基苯甲酸酯 ( Methyl Paraben, Ethyl Paraben, Propyl Paraben 與 Butyl Paraben )。研究中以脂肪酸類化合物作為偽溶劑,當脂肪酸溶解於 鹼性溶液中呈現離子態,具有界面活性劑性質,而當溶液 pH 值下降至 pKa 以下時,脂肪酸呈現分子態,此時則具有有機溶劑性質。萃取過程於 水樣中加入少量的氨水使水溶液成鹼性,再加入有機酸進行皂化反應, 形成界面活性劑,利用為雲點萃取。之後加入適量的硫酸,使當為界面 活性劑之有機酸皂被中和轉成為分子態,產生分散雲團現象。離心後, 取出上層 10μL 脂肪酸注入 HPLC-UV 中進行偵測。為了求得此方法的 最佳萃取條件,分別對脂肪酸,脂肪酸的體積,氨水的體積,硫酸的體 積,鹽類添加量等進行探討。研究結果顯示,在 5 mL 水樣中加入 30μL 的氨水與 40μL 的庚酸,混合均勻進行萃取後,加入 15% 的 NaCl,並 加入 600μL 的硫酸即可獲得最佳的萃取效果。在最佳條件下分析四種對 羥基苯甲酸酯,其線性範圍介於 0.01 ~ 8 μg/mL,線性相關係數高於 0.9980,偵測極限小於 0.008 μg/mL,定量極限小於 0.003 μg/mL,RSD 低於 6.3%。將本方法應用在真實樣品中回收率為 92.2% ~ 104.1%。本開 發方法之分析過程僅使用數微升的脂肪酸及常見的酸與鹼,所使用之材 料不會造成環境負擔,為一操作簡單、方便、快速與高效率,且兼具環 保的綠色化學分析方法。zh_TW
dc.description.tableofcontents謝誌 ........I 摘要 ........II Abstract........III 目錄 ........IV 圖目錄 ........VIII 表目錄 ........IX 第一章 緒論 ........1 1.1 前言 ........1 1.2 Parabens 簡介........1 1.3 雲點萃取法概論 ........4 1.3.1 界面活性劑簡介 ........4 1.3.2 雲點萃取法 ........8 1.4 常見之 Parabens 樣品前處理技術 ........12 1.4.1 液液萃取法 (Liquid-liquid extraction, LLE) ........12 1.4.2 固相萃取法 (Solid phase extraction,SPE) ........13 1.4.3 超臨界流體萃取法 ( Supercritical fluid extraction,SFE ) 15 1.4.4 均相液液萃取法 ( Homogenous liquid-liquid extraction, HLLE ........16 1.4.5 固相微萃取法 ( Solid-phase microextraction,SPME ) .... 18 1.4.1 雲點萃取法 ( Cloud point extraction,CPE )5 ........21 1.5 有機酸雲點微萃取法 ( Pseudo-solvent cloud point microextraction, PS-CPME ) ........21 1.6 研究目的 ........22 第二章 研究方法 ........23 2.1 藥品、器材及儀器設備 ........23 2.1.1 藥品 ........23 2.1.2 器材 ........23 2.1.3 儀器設備 ........24 2.2 藥品配製 ........25 2.2.1 pH7 動相沖提液的配製 ........25 2.2.2 標準品配置........25 2.2.3 MP、EP、PP、BP 檢量線範圍濃度溶液配製........26 2.2.4 直接檢測於洗髮乳之配製 ........26 2.2.5 家庭廢水之取樣及處理........26 2.2.6 添加方法於真實樣品之配製 ........27 2.2.7 添加方法於家庭廢水之配製 ........27 2.3 玻璃裝置之矽烷化........27 2.4 儀器設計及操作條件 ........28 2.4.1 高效能液相層析之參數 ........28 2.4.2 有機酸雲點微萃取系統參數 ........28 2.5 實驗裝置與步驟 ........28 2.5.1 玻璃萃取裝置 ........28 2.5.2 有機酸雲點微萃取法偵測水樣中 Parabens ........28 2.6 有機酸雲點微萃取法最佳條件之探討 ........32 2.6.1 萃取溶劑之選擇........32 2.6.2 萃取溶劑之體積 ........32 2.6.3 Ammonia solution 的體積........33 2.6.4 H2SO4 的體積 ........33 2.6.5 氯化鈉添加量 ........33 2.7 有機酸雲點微萃取法之確效性........34 2.7.1 直接注入校正曲線 ........34 2.7.2 經有機酸雲點微萃取法校正曲線........34 2.8 真實樣品之分析與回收率........35 2.8.1 洗髮乳樣品之分析 ........35 2.8.2 洗髮乳樣品之回收率測定 ........35 2.8.3 家庭廢水樣品之分析 ........35 2.8.4 家庭廢水樣品之回收率測定 ........35 第三章 結果與討論 ........36 3.1 研究內容與架構 ........36 3.2 檢測儀器之最佳條件探討 ........36 3.2.1 動相溶液的選擇........36 3.2.2 UV 偵測波長的選擇 ........36 3.3 有機酸雲點微萃取法最佳條件探討 ........39 3.3.1 萃取溶劑之選擇 ........39 3.3.2 Heptanoic acid 體積之影響 ........42 3.3.3 Ammonia solution 添加量之影響 ........45 3.3.4 H2SO4 添加量之影響........45 3.3.5 NaCl 添加量(鹽析作用)之影響 ........47 3.4 方法可行性評估 ........50 3.4.1 直接注入四種 Parabens 化合物標準品於 HPLC-UV 分析50 3.4.2 以有機酸雲點微萃取法萃取水中四種 Parabens 化合物並經 HPLC-UV 分析 ........50 3.4.3 濃縮倍率 ........51 3.4.4 真實樣品之測定........54 3.4.5 有機酸雲點微萃取與其他萃取方法比較 ........62 第四章 第五章 結論 ........64 參考文獻 ........65zh_TW
dc.language.isozh_TWzh_TW
dc.rights不同意授權瀏覽/列印電子全文服務zh_TW
dc.subjectPseudo-solventen_US
dc.subjectCloud point microextractionen_US
dc.subjectShampooen_US
dc.subjectParabensen_US
dc.subjectHPLC-UVen_US
dc.subject有機酸雲點微萃取zh_TW
dc.subject洗髮乳zh_TW
dc.subjectParabenszh_TW
dc.subject高校液相層析儀-紫外光偵: 測器zh_TW
dc.titleNovel Pseudo-Solvent Based Cloud-Point Microextraction for the Rapid Determination of Parabens in Aqueous Samples by HPLC-UVen_US
dc.title以新型有機酸雲點微萃取法結合 HPLC-UV快速分析水樣中 Parabens 含量zh_TW
dc.typeThesis and Dissertationen_US
dc.date.paperformatopenaccess2018-07-16zh_TW
dc.date.openaccess10000-01-01-
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