Please use this identifier to cite or link to this item: http://hdl.handle.net/11455/16604
標題: 以中空纖維支撐液相微萃取結合液相層析-螢光偵測分析樣品中烷基苯酚
Determination of alkylphenols in environmental sample using hollow fiber protected LPME by HPLC-FLD
作者: 許宗洲
Shiu, Tzung-Jou
關鍵字: Alkylphenols
烷基苯酚
LPME
Hollow fiber
HPLC/FLD
液相微萃取
中空纖維管
出版社: 化學系所
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摘要: 烷基苯酚(alkylphenol)是一種常被使用於塑膠或橡膠中的塑化劑、抗氧化劑及界面活性劑。本身的毒性並不高,然而其結構與雌性激素類似,會干擾原本的內分泌機制,因此在研究與環境觀察中已被證實為環境荷爾蒙,且烷基苯酚容易經由環境中生物的累積及生物降解,存在於大自然的環境中造成環境之危害。 由於文獻分析方法往往需要步驟繁瑣的前處理方法,不但費時且皆需要耗用大量有機溶劑,本研究開發利用中空纖維液相微萃取技術偵測烷基苯酚,不但可以減少有機溶劑使用及前處理步驟,而且可以降低基質干擾。 本實驗探討利用中空纖維支撐液相微萃取技術結合高效液相層析-螢光偵測系統分析環境樣品中烷基苯酚之可行性。實驗中探討液相微萃取之前處理條件(萃取溶劑、萃取時間、萃取攪拌速率、pH值影響、鹽類添加及層析條件),以尋求最佳條件來進行分析物之測定。根據實驗結果顯示以HF-LPME/FLD方法分析環境樣品中烷基苯酚之最佳條件為:萃取溶劑Bromooctane、萃取時間20分鐘、萃取攪拌速率400rpm、pH值調整為6.0、鹽類添加10%NaCl。以利用螢光偵測器(λex=222nm,λem =300nm)分析烷基苯酚類,其線性範圍位於1ng/mL~100ng/mL (butylphenol)和2ng/mL ~200ng/mL (octylphenol、nonylphenol),偵測極限為0.8ng/mL (butylphenol)、0.5ng/mL (octylphenol、nonylphenol)。且利用該方法來偵測環境中工業廢水及聚乳酸生物可分解材質(Polylactic acid, PLA)免洗塑膠杯之烷基苯酚可得到良好的再現性及回收率。
Alkylphenol is a kind of plasticizer and anti-oxidant of plastics and rubber and effective non-ionic surfactant utilized in domestic detergents and cleaners. The toxicity of alkylphenol is not very high, however its structure is similar to natural estrogen. It can result in the disruption of several processes by interfering with the signals that control the overall physiology of the organism. So researches have testified that alkylphenol is the environmental hormones. And alkylphenols easily exist in environment by biodegradation and bioaccumulation. Because the conventional analytical method always need complicated pretreatment steps and larges quantity of organic solvent. In this study, hollow fiber protected liquid phase microextraction is applied as pretreatment step for the determination of alkylphenols in environment samples. This method not only used less organic solvent and simplified operation steps, but also decreased interferes from matrix. In this study, we wanted to confirm the practicability of using HF-LPME/HPLC-FLD to determine alkylphenol in environment samples. In order to find the best conditions to determine analytes, we confirmed pretreatment conditions included extraction solvent, extraction time, stirring speed, effect of pH value and effect of salting out. Results indicated that the optimal sampling conditions as with bromooactane in hollow fiber to collect analytes of 25mL sample solution (with 10% sodium chloride and pH value was controlled to 6.0) at 400 rpm stirring for 20 mins, and then was determined by fluorescence detector. Under the optimal condition, the detection were in the concentration of 1~100 ng/mL for butylphenol, and is at 2~200 ng/mL for octylphenol and nonylphenol. The detection limited were 0.8 ng/mL for butylphenol, and 0.5 ng/mL for octylphenol and nonylphenol. Besides we obtained good reproducibility and recovery when using this method to determine analytes in the wastewater of the factory and the plastics cup of PLA.
URI: http://hdl.handle.net/11455/16604
其他識別: U0005-1507200718211300
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