透過您的圖書館登入
IP:18.118.164.151
  • 學位論文

以垂直震盪器輔助離子液體分散式液液微萃取法分析環境水樣中的苯酮類防曬化合物

A new device for up and down shaker assisted ionic liquid based dispersive liquid-liquid microextraction of benzophenone-type UV filters in environmental water samples

指導教授 : 黃賢達

摘要


由於環境變遷,地球臭氧層遭破壞,太陽紫外線直接對生物體相當大的影響,為了避免紫外光的傷害,人類大量製造及使用防曬產品,所製造的防曬產品使用UV-filters化合物,而防曬產品為現在新興汙染物─藥物與個人護理產品的其中一種,因此開始發展分析方法來偵測環境樣品中的汙染物。目前許多對環境樣品中微量汙染物的樣品前處理技術,如液相─液相微萃取,使用具有揮發性的有機溶劑、不僅有毒還具易燃等性質。本實驗使用離子液體取代了揮發性的有機溶劑;離子液體為近幾年來新興的溶劑之一,也被視為綠色溶劑,廣泛使用在各種研究中,其特性包含熱穩定性佳、不易燃及低蒸氣壓等特性,故應用於分散式液液微萃取的萃取試劑。 本篇研究是以咪唑類的離子液體作為萃取溶劑,使用上下垂直震盪輔助分散式液液微萃取法搭配極致效能液相層析儀,簡單快速的前濃縮步驟萃取水中UV-filters的苯酮類化合物。探討萃取效率之實驗條件有:萃取溶劑和分散溶劑的種類與體積、垂直震盪萃取時間、水樣酸鹼度、鹽類添加與離心的時間的影響。 實驗結果得到最佳化條件為萃取溶劑為[C8MIM][PF6] 離子液體40 μL、分散溶劑為甲醇200 μL、垂直震盪萃取3分鐘、水樣調整於pH7、不加鹽及以轉速5000 rpm離心3分鐘,最後萃取溶劑剩20 μL。本實驗萃取方法之線性範圍為2~1000 ng mL-1,線性濃度相關係數皆大於0.9993。對於游泳池水和汙水處理池廢水之相對回收率為92~120%,相對標準偏差在2.3 ~ 7.1%。在同一天的實驗相對標準偏差(n=3)在1.0~2.9%,而在不同天的實驗標準偏差(n=7)在1.0~2.1%之間。

並列摘要


UV –filters are applied to sunscreen, cosmetic and other personal care products to filter radiation from sunlight. The excessive use of UV filters has led to their presence in the environmental water. A user-friendly ionic liquid –based up and down shaker assisted dispersive liquid-liquid microextraction was develpoed to preconcentrate trace amounts of UV-filters (i.e., benzophenone, 2-Hydroxy-4-methoxybenzophenone, 2,2'-Dihydroxy-4-methoxybenzophenone) from real water sample prior to analysis by ultra performance liquid chromatography (UPLC) combined with PDA . This studied variables were extractant, dispersant, shaking time, salt effect, pH effect, centrifugation time. The optimized experimental conditions were 40 μL [C8MIM][PF6], 200 μL methanol, up and down shaking for 3 mins , NaCl free, adjusted to pH 7, 5000 rpm agitation speed for 3mins. The detection limits of the method ranged from 2~1000 ng mL-1 and the R2 ≥ 0.9993. Recovery studied from different types of real water samples ranged between 92 and 120%.

參考文獻


5. Zhao, L.; Lee, H. K. J. Chromatogr. A 2001, 919, (2), 381-388.
6. Shen, G.; Lee, H. K. Anal. Chem. 2001, 74, (3), 648-654.
9. Jiang, X.; Lee, H. K. Anal. Chem. 2004, 76, (18), 5591-5596.
11. Quina, F. H.; Hinze, W. L. Ind. Eng. Chem. Res. 1999, 38, (11), 4150-4168.
17. Tsai, W.-C.; Huang, S.-D. J. Chromatogr. A 2009, 1216, (27), 5171-5175.

延伸閱讀