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  • 學位論文

手搖輔助超音波增強乳化液液微萃取分析水樣中的內分泌干擾酚類

Analysis of endocrine-disrupting phenols in water samples by shake-assisted ultrasound-enhanced emulsification liquid-liquid microextraction

指導教授 : 黃賢達
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摘要


本文發展了簡單且快速平衡的液相微萃取技術,以手搖輔助超音波增強乳化液液微萃取(SAUELLME)結合極致效能液相層析儀(UPLC)搭配UV偵測器,前濃縮及分析在海水與清潔劑中的五種內分泌干擾酚類(EDPs)。 五種研究的內分泌干擾酚類為4-第三丁基苯酚(4-t-BP)、4-肉桂苯酚(4-CP)、4-第三辛基苯酚(4-t-OP)、2,4-雙丁基苯酚(2,4-di-t-BP)與壬基苯酚(4-NP)。 在手搖輔助超音波增強乳化液液微萃取法(SAUELLME)中,藉由初步的手搖輔助使低密度的有機萃取溶劑形成細小的液滴且乳化分散於水樣中,呈現霧狀。接著超音波震盪使溶液中的細小液滴形成更微小的液滴,藉此增加接觸表面積,以達到提升萃取效果並且更快地萃取分析物達到平衡。 探討了不同的最佳化參數,最佳化後的條件為:有機萃取溶劑為25 μL的一溴十六碳,5 mL的水樣,1分鐘的超音波萃取時間,10秒鐘的手搖輔助時間,離心3分鐘5000 rpm,鹽類的添加為1 g的氯化鈉,沒有pH值的改變,玻璃離心管平躺放置在超音波震盪器正中央。 線性濃度範圍的相關係數皆大於0.995。此方法對於海水的偵測極限是0.5 到2.8 ngmL-1,定量極限是1.8 到9.3 ngmL-1,相對標準偏差的範圍介於4.2 % 到 10.3 %。此方法對於清潔劑的偵測極限是0.4 到2.4 μgmL-1,定量極限是1.6到 8.2 μgmL-1,相對標準偏差的範圍介於4.7 % 到 10.0 %。 在海水水樣與清潔劑水樣中添加分析物測試本實驗的方法是否會受到基質干擾。對於海水的相對回收率為96到109 %,對於清潔劑水樣的相對回收率為81到106 %。

並列摘要


A simple and fast equilibrium liquid-phase microextraction method based on shake-assisted ultrasound-enhanced emulsification liquid-liquid microextraction (SAUELLME) technique combined with ultra performance liquid chromatography (UPLC) with UV detection was developed for the preconcentration and determination of five endocrine-disrupting phenols (EDPs) in seawater samples and detergent samples. The EDPs studied were 4-tert-butylphenol (4-t-BP), 4-cumylphenol (4-CP), 4-tert-octylphenol (4-t-OP), 2,4-di-tert-butylphenol (2,4-di-t-BP) and 4-nonylphenol (4-NP). For SAUELLME, dispersion of the fine droplets of a low density organic extraction solvent into the aqueous sample is formed by use of the first step shake- assisted for mixing, and then the fine droplets could extract target analytes toward equilibrium faster because of the shorter diffusion distance and larger surface area by ultrasound-enhanced emulsification. Different experimental parameters were controlled and the optimum conditions found were: 25 μL of 1-bromohexadecane as the extraction solvent, 5 ml water samples, 1 minute ultrasound extraction time, 10 seconds shake-assisted time, centrifugation for 3 min at 5000 rpm, 1g NaCl for ionic strength, no pH adjustment, centrifugation tube was lying on the center of ultrasonic bath system. The correlation coefficient (γ2 ) greater than 0.995 for calibration curve range. The limit of detection (LOD) was 0.5 to 2.8 ngmL-1, the limit of quantitation (LOQ) was 1.8 to 9.3 ngmL-1 and the relative standard deviation (RSD) ranged from 4.2 % to 10.3 % for seawater samples. The limit of detection (LOD) was 0.4 to 2.4 μgmL-1, the limit of quantitation (LOQ) was 1.6 to 8.2 μgmL-1 and the relative standard deviation (RSD) ranged from 4.7 % to 10.0 % for detergent samples. Applying proposed method to spiked seawater samples and detergent samples in order to determine matrix effects. The relative recovery was 96 % to 109 % for seawater samples and 81 % to 106 % for detergent samples.

參考文獻


[12] 特殊健康危害專題季刊,發行單位:行政院衛生署國民健康局;編輯單位:國立成功大學,2010
荷爾蒙物質管理及環境流布調查”,行政院環境保護署環境檢驗所
[8] 林維雋,“以一維及二維氣相層析質譜儀檢測生物檢體中烷基酚之分析與研究”,2007,國立中央大學化學研究所碩士論文
[25] 劉智豪,“以微量溶劑冷凝分散液液微萃取法偵測水中烷基苯酚化合物”,2010,國立清華大學化學研究所碩士論文
[34] A.-L. Theis, S.-M. Hansen, M.-A. Jeannot, Anal.Chem., 73 (2001) 5651

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