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研究生:李文彥
研究生(外文):Wen-yan Lee
論文名稱:線上固相萃取結合親水作用液相層析質譜儀檢測河水中四級銨類農藥
指導教授:傅明仁
指導教授(外文):Ming-ren Fuh
學位類別:碩士
校院名稱:東吳大學
系所名稱:化學系
學門:自然科學學門
學類:化學學類
論文種類:學術論文
論文出版年:2010
畢業學年度:99
語文別:中文
論文頁數:135
中文關鍵詞:線上固相萃取親水作用層析質譜農藥
外文關鍵詞:online speHILICMSquaternary ammonium herbicides
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四級銨類農藥包含除草劑與植物生長調節劑,不論在國內外都使用相當普遍,活性成分都是典型的小分子化合物,容易附著在土壤內或是農作物表面,與水極為相溶,也因為如此常存於環境中水樣。在各國法規上,歐盟 (EU) 於農作物產品中規定單一農藥存在的最大值不得超過0.05 mg/Kg,而對環境水,歐盟並沒有針對四級銨類農藥有詳細規範,但是規定個別的農藥含量需少於0.1μg/L,總體的農藥含量最多不得超過0.5μg/L;美國環境保護局 (USEPA) 則是規範飲用水中Paraquat及Diquat最大值分別為0.02 mg/L、0.03 mg/L,台灣食品藥物管理局則是對Paraqaut在各種疏果食品規範由0.01 mg/L至0.5 mg/L不等,為了持續規範更詳盡之相關法規,分析四級銨類農藥之方法仍然是不可或缺的。
本研究的目的就是在開發出一套利用線上固相萃取結合親水作用液相層析/電灑/質譜儀來檢測河水中四級銨類農藥的方法,由於固相萃取的樣品前處理技術能有效地去除河水中的基質干擾,再加上我們將此技術轉移至線上,河水樣本可藉由簡單的過濾裝置後直接注入線上固相萃取連結親水作用液相層析/電灑/質譜儀系統中進行檢測,此方法對溪水中分析物在5ng/ml~500ng/ml 之間均有良好的線性關係,偵測極限約在2.5ng/ml~5ng/ml,其inter-day及intra-day實驗之精確度誤差在0.8%~14.1%之間,準確度在96.7%~110.7%之間,回收率在95.6%~108.0%。
中文摘要 頁次
第一章 緒論 1
第一節 四級銨類農藥之介紹 1
第二節 常見分析四級銨類農藥之方法 6
第三節 固相萃取法 8
第四節 線上固相萃取結合親水作用液相層析/電灑
/質譜儀檢測河水中四級銨鹽類農藥 12
第五節 親水作用液相層析/電灑/質譜儀的應用與
發展 13
第六節 離子阱質譜儀 18
第二章 實驗部份 22
第一節 樣品及試劑 22
第二節 儀器及設備 22
第三節 實驗架構及步驟 26
第三章 結果與討論 39
第一節 離子阱質譜儀部分 39
1. 質譜儀毛細管出口端電壓對訊號強度的影響 39
2. 前趨離子之文獻比較 41
3. 質譜儀斷裂電壓對訊號強度的影響 44
第二節 線上固相萃取連接親水作用液相層析管柱 55
2-1. 親水作用液相層析管柱條件之測試 55
(1). 親水作用液相層析管柱之梯度找尋 55
(2). 移動相鹽類的添加對分析物訊號與峰寬的影響 55
2-2. 分析物光降解之測試 65
2-3. 線上固相萃取管柱連接親水作用液相層析管柱
條件之測試 65
(1). 線上固相萃取管柱進樣液pH值之探討 70
(2). 線上固相萃取管柱沖洗液濃度之探討 74
(3). 固相萃取管柱與親水作用液相管柱連接之相
容性 74
(4). 注入的樣品體積探討 78
第三節 河水基質效應探討 84
1. 河水樣基質效應之探討 84
2. 基質效應對線性的影響 92
3. 固相萃取回收率之測試 92
第四節 偵測極限與線性關係 98
1. 靈敏度及偵測極限 98
2. 線性關係 98
3. 精確度與準確度之測試 98
第五節 真實樣品 105
1. 真實河水樣之檢測 105
第六節 結論 109
第四章 參考文獻 111
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