Please use this identifier to cite or link to this item: http://hdl.handle.net/11455/16831
標題: 超音波輔助乳化微萃取技術結合GC-ECD快速分析環境水樣與土壤中有機磷農藥之開發
Developments of ultrasound-assisted emulsification microextraction for the rapid analysis of organophosphorus pesticides for environmental water and soil samples using gas chromatography-electron capture detector
作者: 蘇奕菘
Su, Yi-Song
關鍵字: Microwave-assisted extraction;微波輔助萃取;Emulsification microextraction;Gas chromatography;Organophosphorus pesticides;乳化微萃取;氣相層析儀;有機磷農藥
出版社: 化學系所
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摘要: 
本研究開發以超音波輔助乳化微萃取之快速綠色採樣濃縮前處理技術,經與氣相層析儀電子捕獲偵測器結合後成功分析檢測水樣與土壤中有機磷農藥的殘留量。針對水中有機磷農藥的採樣,本研究以自製裝置大幅改進萃取後萃取劑收集的方便性,萃取過程使用玻璃針筒為樣品處理容器,置入水樣後添加極微量(數微升)的低密度有機溶劑作為萃取採樣溶劑,經套封後,隨即放入超音波水漕中震盪,使有機溶劑乳化分散於水樣中進行微萃取,經高速離心分層後,解開套封接上推栓與自修改加刻度的微細玻璃管,將上層有機溶劑推至微細玻璃管中,取有機溶劑注入GC-ECD中進行分離與偵測。研究中對水樣所探討的條件包括:有機溶劑的選擇、萃取溶劑的添加量、超音波輔助乳化的時間、溶液pH值、鹽析效應等。最佳化參數為添加20μl的甲苯有機溶劑於pH 8的水樣中,超音波照射30秒,離心3分鐘,整體操作時間4-5分鐘即可完成。另外,對土壤中有機磷農藥採樣,使用實驗室自行改裝微波輔助萃取裝置,以水為萃取劑對環境土壤樣品進行採樣,並結合上述之超音波輔助乳化微萃取技術予以濃縮。對環境土壤樣品所探討的條件包括:微波功率、微波時間、水量、有機修飾劑對萃取效率之影響。最佳化參數為微波照射功率226瓦、時間2.5分鐘,結合超音波輔助乳化微萃取技術濃縮,整體操作時間8-9分鐘即可完成。驗證本研究方法的可行性,應用此技術於真實樣品中有機磷農藥之測定,成功檢測出農田廢水與土壤中微量的有機磷農藥殘留。為一實驗裝置簡單、操作簡便、便宜、快速且不需使用大量有機溶劑的綠色前處理方法。

A simple, efficient and novel pretreatment technique termed as ultrasound-assisted emulsification microextraction (USAEME) has been designed and studied for the rapid analysis of organophosphorus pesticides (OPPs) in environmental water and soil samples by gas chromatography-electron capture detector (GC-ECD). A specially designed extraction device was utilized for the facilitated collection of extraction solvent from the extraction unit for the extraction of OPPs in water and soil sample matrixes. A glass syringe as an extraction unit, a microsyringe for extractant addition, and a self-scaled glass capillary tube adopted onto the needle holder of the glass syringe as a means to recover the extractant. A trace amount (few μl) of low-density organic solvent as the extraction solvent was added into the aqueous sample solution followed by the ultrasonic radiations which accelerate the emulsification of μL-level solvent in aqueous solution to enhance the microextraction efficiency of OPPs. The formed emulsion was centrifuged and the amount of separated organic extract was measured in the self-scaled glass capillary tube and then 1 μL of organic extract was directly injected into a GC-ECD for analysis. Parameters affecting the extraction efficiency of OPPs in aqueous samples such as selection of organic extraction solvents, volume of extraction solvent, ultrasound-assisted emulsification time, pH of the sample solution, addition of salt to sample solution were thoroughly investigated. Results showed that the optimum extraction efficiency of OPPs in 5 mL of aqueous sample (pH = 8) by the addition of 20 μL toluene as the extraction solvent, followed by ultrasonication for 30 seconds and then centrifugation for 3 min at 3200 rpm.
An upgraded microwave-assisted extraction (MAE) was coupled with USAEME and applied for the extraction of OPPs in soil samples using water as an extraction medium. Microwave irradiation was utilized to accelerate the extraction of OPPs from soil sample into water medium. Parameters affecting the extraction efficiency of OPPs in soil such as selection of the power and irradiation time of microwave, volume of extraction medium (water) were investigated. Results showed that the optimum extraction efficiency of OPPs in soil matrix was obtained by the microwave irradiation of sample solution at optional pH 8 with the irradiation power of 226 Watt for 2.5 min. MAE coupled with USAEME showed higher extraction efficiency under the extraction time of 8-9 minutes for the extraction of OPPs in soil samples. In order to verify the applicability, the proposed methods were successfully applied for OPPs determination in agricultural water and soil samples. The proposed methods provided a simple, cheap, fast and eco-friendly procedure for the sampling of OPPs from complicated sample matrix.
URI: http://hdl.handle.net/11455/16831
其他識別: U0005-2807201015353600
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