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標題: Salt-assisted homogenous extraction followed by subcritical water chromatography for the determination of parabens in cosmetic products
作者: 林巧雯
Lin, Chiao-Wen
關鍵字: salt-assisted homogeneous liquid liquid extraction;鹽類輔助均相萃取;subcritical water chromatography;parabens;次臨界水層析法;Parabens
出版社: 化學系所
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In 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.

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。
其他識別: U0005-2707201111421900
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