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dc.contributorMaw-Rong Leeen_US
dc.contributor.advisorJen-Fon Jenen_US
dc.contributor.authorLin, Chiao-Wenen_US
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dc.description.abstractIn this study, salt-assisted homogeneous liquid liquid extraction (SHLLE) followed by subcritical water chromatography (SBWC) for determination of preservatives including Methyl paraben (MP), Ethyl paraben (EP) , Propyl paraben (PP) in cosmetic products. For convenience in quantifying the collected solvent, the present work utilizes a self-designed glass container in the extraction process. The optimum parameters for SHLLE and SBWC of MP, EP and PP were investigated. The best results of extraction process were obtained as follows: To 5 ml liquid sample adjusted to pH 6, added 200μl Isopropanol as the extraction solvent followed by 4 g of ammonium sulfate as the phase separation agent. After phase separation, the upper layer containing the extraction solvent was collected and dried by moderate nitrogen, dissolved in water of pH 10.5 and injected into subcritical water chromatograph. The optimum results of SBWC were obtained by using PLRP-S (100A 5μm, 15 cm × 4.6 mm I.D.) column with pH 10.5 citric acid buffer as mobile phase. The temperature of the preheater and column oven were set as 80oC and 100oC respectively. Under these conditions, the liner range was 0.75-75 μg/L for MP, EP and 1.5-150 μg/L for PP with RSD below 9.2%. Detection limits were achieved at level of 0.07~0.1 μg/L. The results demonstrated that the proposed method was a simple, inexpensive and eco-friendly approach for the determination of paraben preservatives in cosmetic products.en_US
dc.description.abstract本研究開發鹽類輔助均相萃取技術結合次臨界水層析進行分離與偵測化妝品中的三種Parabens。使用自行設計的玻璃容器當作萃取裝置,並利用可與水互溶的萃取試劑,均相萃取後再加入硫酸銨鹽,輔助相的分層,經離心分層後,使上層的萃取溶劑經由容器上之刻度直接定量並取出,將取出的萃取溶劑利用氮氣吹乾後再以10 μL的水回溶進入次臨界水-UV系統進行偵測。在次臨界水系統中分離偵測三種Parabens,使用動相pH 10.5的緩衝溶液、管柱加熱器100℃、UV波長296 nm,有最佳的層析效果。而在鹽輔助均相萃取技術,為了求得此方法的最佳化條件分別對萃取溶劑、萃取溶劑的體積、硫酸銨鹽的添加量和水樣的pH值等參數進行探討。實驗結果發現,在5毫升pH 6的水樣中,加入200 μL的Isopropanol,並添加4克的硫酸銨鹽攪拌至飽和可獲得最佳的萃取效果。Parabens在經由方法最佳條件下濃縮倍率為238~309之間,偵測極限為0.07~0.1μg/L之間。將本方法應用在真實樣品中回收率為92.3% ~ 109.6%。整個實驗方法與分析過程僅需要數百微升的有機溶劑,是一個方法裝置簡單、快速的綠色化學分析法。zh_TW
dc.description.tableofcontents謝誌 I 摘要 II Abstract III 目錄 IV 圖目錄 VI 表目錄 VII 第一章 緒論 1 一、 前言 1 二、 次臨界水層析法概論 3 (一) 次臨界水的性質 3 (二) 次臨界水文獻回顧 9 三、 Parabens簡介-生活用品中的防腐劑 19 四、 常見的Parabens樣品前處理技術 22 (一) 液液萃取法 ( Liquid-liquid extraction,LLE ) 22 (二) 超臨界流體萃取法 ( Supercritical fluid extraction,SFE ) 23 (三) 固相萃取法 ( Solid phase extraction,SPE ) 24 (四) 固相微萃取法 ( SPME ) 25 (五) 均相液液萃取法 29 五、 研究目的 35 第二章 實驗材料與研究方法 36 一、 藥品、器材及儀器設備 36 (一) 藥品 36 (二) 器材 37 (三) 儀器設備 37 (四) 儀器裝置圖 38 (五) 玻璃萃取裝置 39 二、 藥品配製 42 (一) 動相沖提液的配製 42 (二) 標準品的配製 43 (三) MP 、EP、PP檢量線範圍濃度溶液的配置 43 (四) 直接檢測於真實樣品的配製 44 (五) 添加方法於真實樣品的配製 44 三、 儀器設計及操作條件 45 (一) 次臨界水層析儀系統參數 45 (二) 鹽輔助均項萃取系統參數 45 (三) 鹽輔助均相萃取法實驗操作步驟 45 (四) 次臨界水層析系統建構 47 (五) 鹽輔助均相萃取最佳化條件之探討 51 (六) 再現性探討與真實樣品測定 53 第三章 結果與討論 54 一、 次臨界水層析法最佳條件探討 54 (一) UV偵測波長的選擇 54 (二) 動相pH值與管柱加熱器的選擇 54 (三) 萃取溶劑在次臨界水層析法中的影響 59 (四) 次臨界水層析系統最佳化條件 59 二、 鹽輔助均相萃取法最佳化條件探討 61 (一) 鹽輔助均相萃取法中萃取溶劑的選擇 61 (二) 鹽輔助均相萃取法中鹽類的選擇 64 (三) 萃取溶劑的體積 65 (四) 鹽類添加量 67 (五) 水樣pH值的影響 67 三、 方法可行性的評估 70 (一) 以直接進樣三種Parabens化合物於次臨界層析系統分析 70 (二) 經由鹽輔助萃取法萃取水中三種Parabens並經由次臨界層析系統中分析 70 (三) 鹽輔助均相萃取法與其他萃取方法比較 72 四、 真實樣品的分析 74 (一) 直接檢測 74 (二) 添加方式檢測 74 第四章 結論 78 第五章 參考文獻 79zh_TW
dc.subjectsalt-assisted homogeneous liquid liquid extractionen_US
dc.subjectsubcritical water chromatographyen_US
dc.titleSalt-assisted homogenous extraction followed by subcritical water chromatography for the determination of parabens in cosmetic productsen_US
dc.typeThesis and Dissertationzh_TW
item.openairetypeThesis and Dissertation-
item.fulltextno fulltext-
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