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研究生:楊曜嘉
研究生(外文):Yang, Yao-Jia
論文名稱:高效能液相層析結合綠色溶劑離子液體微萃取分析食品中動物性用藥之研究
論文名稱(外文):Analysis of Drugs in Food Producing Animals by HPLC through Green Solvent Ionic Liquid Microextraction
指導教授:喻家駿
口試委員:瞿港華林昭任
口試日期:2013-07-22
學位類別:碩士
校院名稱:逢甲大學
系所名稱:環境工程與科學學系
學門:工程學門
學類:環境工程學類
論文種類:學術論文
論文出版年:2013
畢業學年度:101
語文別:中文
論文頁數:107
中文關鍵詞:離子液體液-液相微萃取食用動物性用藥氯黴素甲磺氯黴素樣品前處理技術萃取效率
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近年來,由於食用性動物之飼養多以密集之方式經營,若導致疾病發生則將會使疾病迅速蔓延。為求生產食用性動物之安全及預防疾病帶來損失,在飼養期間使用抗生素和藥品來預防和治療食用性動物之疾病,間接地導致這些抗生素和藥品殘留於食用性動物的體內,食入後將影響人類的健康。因此為了保障人類的健康安全,對於環境樣品之檢測分析必須要有更高的準確性和精確性在分析檢測樣品中微量之食用動物性用藥,樣品的前處理技術提供了將樣品消除基質干擾,提高方法的準確度、精確度、選擇性和靈敏度,在液-液相萃取法中有機溶劑的使用具有其揮發性毒性,對環境和人類皆有危害,因此離子液體(Ionic liquids, ILs)萃取法為近代發展出一種新型、綠色、無毒、靈敏的樣品前處理技術。
本研究實驗以離子液體(1-丁基-1-甲基吡咯啶雙(三氟甲基磺醯基)醯亞胺) [BMPy][Tf2N]結合高效能液相層析儀(HPLC)檢測分析食用性動物用藥氯黴素(CAP)和甲磺氯黴素(TAP)之殘留,比較離子液體[BMPy][Tf2N]及有機溶劑乙酸乙酯、二氯甲烷對CAP及TAP之萃取效率,分析最佳條件為以紫外光偵測分別以氯黴素278nm和甲磺氯黴素224nm進行檢測,沖提液為氰甲烷和去離子水(30/70, V/V),流速為1.5mL/min,氯黴素和甲磺氯黴素之方法偵測極限(MDL)各為0.095mg/L和0.120mg/L,檢量線之相關係數為0.9996和0.9958。實驗結果顯示,以離子液體[BMPy][Tf2N]萃取分析氯黴素和甲磺氯黴素之低濃度樣品,可達最佳萃取效率為97%以上。應用於環境樣品中,添加微量之氯黴素和甲磺氯黴素混合溶液,以離子液體[BMPy][Tf2N]萃取分析,可達最佳萃取效率為95%以上。與有機溶劑乙酸乙酯和二氯甲烷萃取效率相比較,有機溶劑的萃取效率較差。因此,本研究實驗結果得知離子液體能應用於檢測分析食用動物性用藥之殘留,也能夠取代揮發性有機溶劑且萃取率高。
In recent years, food-producing animals is intensive feeding, so animals diseases caused by rapid. For the safety and prevention of food-producing animals, use of the antibiotics and drugs to prevent and treat the disease of food-producing animals during the rearing period, it may lead to residue of antibiotics and drugs in food-producing animals in vivo, Ingestion will affect human health. Therefore, in order to protect human health and safety, for the detection and analysis of environmental samples must be higher accuracy and precision in the analysis of trace detection of drug use in food-producing animals. Sample pretreatments technology has eliminated the sample matrix interference, improve accuracy of the method, accuracy, selectivity and sensitivity, organic solvents are volatile and toxic in the liquid-liquid extraction method, exposure to those hazardous materials can cause severe harmful to human body and environment. Ionic liquids (ILs) are a novel, green, non-toxic and sensitive samples pretreatment technique.
In this study, the chloramphenicol (CAP) and thiamphenicol (TAP) drugs in food-producing animals were extracted by ionic liquid [BMPy][Tf2N] i.e. 1-butyl-1-methylpyrrolidinium-bis(trifluoromethylsulfonnyl)imide from aqueous solution. The comparisons of the extraction solvents of [BMPy] [Tf2N], ethyl ethanoate and dichloromethane were carefully evaluated. The extracted samples were analyzed by a high performance liquid chromatography (HPLC) with the detection wavelength CAP 278nm, TAP 224nm, and the mobile phase of a mixture of acetonitrile/pure water (30/70, V/V). The method limit of detection (MLD) of chloramphenicol and thiamphenicol was 0.095 mg/L and 0.120 mg/L, respectively. The correlation coefficients of calibration curve were 0.9996 and 0.9958 respectively. The experimental results show the extraction low concentration samples of chloramphenicol and thiamphenicol by ionic liquid [BMPy][Tf2N], the best extraction efficiency reaches 97%. The method was applied to analyze the environmental samples with limited concentration; the best extraction efficiency reaches 95%. Organic solvent extraction efficiency is low by comparison of ionic liquids with organic solvents. Accordingly, the experimental results have proven that ionic liquids could not only extraction low concentration of drugs in food-producing animals and have high effective extraction, also could replace the toxic organic solvents.
中文摘要 ...............................i
英文摘要 ..............................ii
目錄 .............................iii
表目錄 .............................vii
圖目錄 ............................viii
第一章 緒論 .......................1
1.1 研究緣起與目的 .......................1
1.2 研究內容 .......................2
第二章 文獻回顧 .......................4
2.1動物性用藥介紹 .......................4
2.2動物性用藥管制標準 ...................6
2.3動物性用藥種類 .......................9
2.4氯黴素類 ......................15
2.4.1氯黴素種類之介紹 ..............15
2.5氯黴素種類之危害 ..............20
2.6氯黴素種類之法規 ..............21
2.7離子液體 ......................23
2.7.1離子液體介紹 ......................23
2.7.2離子液體種類 ......................24
2.7.3離子液體特性 ......................29
2.7.3.1熔點 ......................30
2.7.3.2黏度 ......................33
2.7.3.3溶解性 ......................34
2.7.3.4熱穩定性 ......................37
2.7.3.5導電度和電化學電位窗 ..............37
2.7.4離子液體之應用 ..............38
2.7.5本實驗所選用之離子液體 ..............40
2.7.6製備合成離子液體[BMPy][Tf2N] ......41
2.8食品檢測分析方法 ..............42
第三章 實驗藥品、設備及方法 ..............44
3.1 實驗藥品 ......................44
3.1.1萃取溶劑 ......................44
3.1.2食品中動物用藥 ..............44
3.1.3環境樣品 ......................45
3.1.4分析藥品 ......................45
3.2標準品配製 ......................45
3.2.1 1000 mg/L標準品儲備溶液 ......45
3.2.2 移動相溶液 ......................46
3.3 環境樣品配製 ......................46
3.4實驗設備 ......................46
3.5實驗流程 ......................47
3.6實驗步驟與方法 ......................49
3.6.1樣品波長之測定 ..............49
3.6.2移動相比例之測定 ..............49
3.6.3製備樣品之檢量線 ..............50
3.6.4方法偵測極限(Method detection limit, MDL)之測定 ......................50
3.6.5離子液體和有機溶劑萃取之步驟 ......52
3.6.6環境樣品之檢測 ..............54
3.6.7萃取回收率之計算 ..............55
第四章 結果與討論 ......................56
4.1分析條件參數之建立 ..............56
4.1.1吸收波長之測定 ..............57
4.1.2沖提溶液之選擇 ..............58
4.2空白樣品分析 ......................59
4.2.1單一樣品之分析 ..............60
4.2.2混合樣品之分析 ..............62
4.3檢量線製作 ......................63
4.4方法偵測極限之測定 ..............68
4.5離子液體萃取分析 ..............70
4.5.1空白分析 ......................70
4.5.2離子液體萃取單一及混合樣品 ......72
4.6有機溶劑之萃取 ......................82
4.7食用動物性用藥殘留萃取分析 ......87
4.8萃取效率之探討 ......................94
第五章 結論 ......................97
第六章 參考文獻 ......................99
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