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研究生:李宏萍
研究生(外文):Li, Hong-Ping
論文名稱:微波輔助頂空固相微萃取技術應用於農藥殘留分析研究
論文名稱(外文):Determination of Pesticides in Water with Microwave Assisted Headspace Solid-Phase Microextraction and Gas Chromatography
指導教授:鄭政峰鄭政峰引用關係
指導教授(外文):jen, Jen-Fon
學位類別:博士
校院名稱:國立中興大學
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:2004
畢業學年度:92
語文別:中文
論文頁數:212
中文關鍵詞:多種農藥同時分析有機氯農藥合成除蟲菊類農藥有機磷劑農藥微波輔助-頂空-固相微萃取
外文關鍵詞:Multiresidue pesticides analysisOrganochlorine pesticides (OCPsPyrethroid pesticides (Pyrs)Organophosphorate pesticides (OPs)Microwave assisted-Headspace-Solid phase microextraction(MA-HS-SPME)
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本研究發展以微波輔助頂空固相微萃取(MA-HS-SPME)新技術應用於農藥分析樣品前處理之研究,配合以快速毛細管氣相層析儀附電子捕獲式檢測器(Fast cGC-μECD)及火焰光量檢測器(GC-FPD)對農藥作分析。研究中就影響萃取的因素如樣品基質修飾、固相微萃取纖維管的選擇、微波功率、微波照射吸附時間、脫附溫度、時間及層析條件等作詳盡探討,求得最佳萃取及分析條件,研究中就本開發技術對農藥的主要分類進行可行性作探討。研究結果顯示對於水中16種有機氯劑農藥的分析以80% (244瓦特)微波功率照射10分鐘,以50/30 μm DVB/CAR/PDMS纖維管吸附,進行MA-HS-SPME萃取再於氣相注入口以310℃ 脫附3分鐘,以cGC-μECD分析,可偵測水中濃度除Endosulfan sulfate為0.25至2.5μg/l外,其餘農藥皆可達0.05至2.5μg/l之間,其檢量線之r2值皆大於0.9978,最低偵測極限可達0.002至0.07μg/l,其相對標準偏差皆小於15%。對於水中10種合成除蟲菊類農藥之分析,以P4 (157瓦特)微波功率照射10分鐘,以100 μm PDMS纖維管進行萃取吸附,再於cGC注入口以290℃脫附3分鐘下,以cGC-μECD進行分析,偵測在水中濃度範圍為0.05-0.5 μg/l,其檢量線之r2值除了畢芬寧0.9812之外,其它均大於0.9913,偵測極限可達0.0002-0.0026 μg/l。對於 水中8種有機磷劑農藥之分析,以80% (244瓦特)微波功率照射15分鐘,以50/30 μm DVB/CAR/PDMS纖維管進行MA-HS-SPME萃取吸附,再於cGC注入口以310℃脫附3分鐘及cGC-FPD分析,偵測濃度範圍為0.5-40 μg/l,其檢量線之r2值大於0.9867,偵測極限可達0.023至1.432 μg/l之間。本方法可應用於環境水體中多種農藥篩檢之檢測,不僅偵測極限均比傳統方法降低2-3級數,此方法可在短時間內完成多種農藥快速篩選,過程中無使用溶劑,是個符合環保需求的檢測方法。
A coupled technique, microwave-assisted headspace solid-phase microextraction (MA-HS-SPME), was investigated for one-step in-situ sample pretreatment for multi-pesticides screening prior to gas chromatographic determination. The pesticides were collected by the proposed method and analyzed by gas chromatography with an electron capture detector (GC-ECD) or flame photometric detector (GC-FPD). To perform the MA-HP-SPME, six types of SPME fibers were examined and compared. The parameters affecting the efficiency in MA-HS-SPME process such as sampling time and temperature, microwave irradiation power, desorption temperature and time were studied to obtain the optimal conditions.
Results showed that the optimum extraction efficiency of OCPs in aqueous matrix was obtained by irradiation of sample solution with irradiation power 244 Watt for 10 min. The detection was linear in the studied concentration range with γ2 > 0.9978. The detection limits varied from 0.002-0.070μg/l. For pyrethroids, irradiation power 157 Watt for 10 min. The detection was linear in the studied concentration range with γ2 >0.9913 except bifethrin. The detection limits varied from 0.0002-0.0026μg/l. For Organophosphate pesticides, OPPs irradiation power 244 Watt for 15 min can get the optimum extraction efficiency. The detection was linear in the studied concentration range with γ2 > 0.9867. The detection limits varied from 0.023-1.432 μg/l. The results indicate that the proposed method provides a very simple, fast, and solvent-free procedure to achieve the sample pretreatment prior to the trace-level screening determination of pesticides by gas chromatography.
目錄
摘 要 I
Abstract II
目錄 III
圖目錄 IX
表目錄 XIII
簡語表 XVI
符號表 XVII
第一章 緒論 2
1-1 研究緣起與目的 2
1-2 研究架構與內容 4
1-3 微波輔助頂空固相微萃取技術之原理 7
1-3-1:微波輔助萃取原理 7
1-3-2:頂空萃取原理 15
1-3-3:固相微萃取原理 16
1-3-3-1固相微萃取纖維管直接液體採樣: 17
1-3-3-2頂空採樣 19
1-3-3-3直接採樣的萃取速率 21
1-3-3-4頂空採樣的萃取速率 21
第二章 分析農藥的基本資料及文獻探討 26
2-1 有機磷劑農藥、有機氯農藥及除蟲菊類農藥基本資料 26
2-1-1有機氯農藥 26
2-1-2 除蟲菊類農藥 26
2-1-3 有機磷劑農藥簡介 27
2-2 文獻探討 28
2-2-1公告之多種農藥殘留檢測方法簡介 28
2-2-2 微波輔助萃取應用於農藥殘留檢測 39
2-2-3 頂空萃取應用於農藥殘留檢測 44
2-2-4固相微萃取應用於農藥殘留檢測 46
第三章 試驗材料及研究方法 54
3-1 藥品及器材 54
3-2 藥品配製 56
3-3 玻璃器皿的矽烷化 70
3-4 氣相層析儀條件之探討 70
3-5 固相微萃取纖維之活化 73
3-6 微波頂空固相微萃取裝置的建立 73
3-7 實驗研究步驟 79
3-7-1 水中有機氯農藥測定 79
3-7-1-1 微波輔助頂空固相微萃取方法 79
3-7-1-2 傳統液液相萃取方法 79
3-7-2 土壤中有機氯農藥測定 80
3-7-2-1 微波輔助頂空固相微萃取方法 80
3-7-2-2 公告土壤中有機氯農藥殘留分析-超音波萃取法(143) 80
3-7-3 水中合成除蟲菊類農藥測定 81
3-7-3-1 微波輔助頂空固相微萃取方法 81
3-7-3-2 固相萃取方法(SPE)(144) 81
3-7-3-3 液液相萃取方法(LLE) 82
3-7-4 水中有機磷劑農藥測定 82
3-7-4-1 微波輔助頂空固相微萃取方法 82
3-7-4-2 液液相萃取方法(LLE) 82
3-7-5 水中多種農藥測定 83
3-7-5-1微波輔助頂空固相微萃取方法 83
3-7-5-2 多種農藥直接注入氣相層析儀檢量線及偵測極限 83
第四章 結果與討論 84
4-1 水中有機氯農藥分析之研究: 84
4-1-1 氣相層析與分離管柱之選擇 84
4-1-2 固相微萃取纖維塗覆種類及厚度選擇之影響 86
4-1-3 固相微萃取纖維之熱脫附條件的建立 88
4-1-3-1 固相微萃取纖維之熱脫附溫度的建立 88
4-1-3-2 固相微萃取纖維之熱脫附時間的建立 88
4-1-4 最佳微波照射條件的建立 91
4-1-4-1 微波照射最佳化功率之選擇 91
4-1-4-2 微波照射時間的選擇 91
4-1-5 萃取液pH選擇的影響 94
4-1-6 鹽類添加的影響 94
4-1-7頂空空間體積 97
4-1-8 有機氯農藥之校正曲線範圍、校正曲線方程式、校正曲線相關係數及偵測極限值 97
4-1-8-1 以直接進樣經GC-ECD分析 97
4-1-8-2 以MA-HS-SPME萃取經GC-ECD分析 100
4-1-9 灌溉水及0.05%腐植酸水以MA-HS-SPME萃取經GC-ECD分析之回收率測定 100
4-1-10微波頂空固相微萃取與液液相/固相萃取方法比較 100
4-1-11 CRM標準水樣品微波頂空固相微萃取與液液相/固相萃取方法比較 101
4-1-12水樣品中有機氯農藥微波頂空固相微萃取與液液相/固相萃取方法秏材比較 101
4-2 土壤中有機氯農藥分析之研究: 108
4-2-1 以MA-HS-SPME萃取經GC-ECD分析 108
4-2-2 田土及含0.05%腐植酸土壤以MA-HS-SPME萃取經GC-ECD分析之回收率測定 108
4-2-3微波頂空固相微萃取與超音波/固相萃取方法比較 108
4-2-4真實土壤樣品中有機氯農藥微波頂空固相微萃取與超音波/固相萃取方法比較 109
4-3 水中合成除蟲菊類農藥分析之研究: 109
4-3-1 氣相層析與分離管柱之選擇 109
4-3-2 固相微萃取纖維塗覆種類及厚度選擇之影響 115
4-3-3 固相微萃取纖維之熱脫附條件的建立 116
4-3-3-1 固相微萃取纖維之熱脫附溫度的建立 116
4-3-3-2 固相微萃取纖維之熱脫附時間的建立 120
4-3-4 最佳微波照射條件的建立 120
4-3-4-1 微波照射最佳化功率之選擇 120
4-3-4-2 微波照射時間的選擇 123
4-3-5 萃取液pH選擇的影響 123
4-3-6合成除蟲菊類農藥之校正曲線範圍、校正曲線方程式、校正曲線相關係數及偵測極限值 128
4-3-6-1 以直接進樣經GC-ECD分析 128
4-3-6-2 以MA-HS-SPME萃取經GC-ECD分析 128
4-3-6-3 地下水添加10種合成除蟲菊類農藥以MA-HS-SPME萃取經GC-ECD分析 128
4-3-7地下水添加10種合成除蟲菊類農藥以三種不同萃取方法經GC-ECD分析之比較 134
4-4 水中有機磷劑農藥分析之研究: 136
4-4-1 氣相層析與分離管柱之選擇 136
4-4-2 固相微萃取纖維塗覆種類及厚度選擇之影響 136
4-4-3 固相微萃取纖維之熱脫附條件的建立 137
4-4-3-1 固相微萃取纖維之熱脫附溫度的建立 137
4-4-3-2 固相微萃取纖維之熱脫附時間的建立 142
4-4-4 最佳微波照射條件的建立 142
4-4-4-1 微波照射最佳化功率之選擇 142
4-4-4-2 微波照射時間的選擇 142
4-4-5 鹽類、溶劑添加的影響 146
4-4-5-1 鹽類添加的影響 146
4-4-5-2溶劑添加的影響 146
4-4-5-3 鹽類、溶劑添加的影響 146
4-4-6有機磷劑農藥之校正曲線範圍、校正曲線方程式、校正曲線相關係數及偵測極限值 146
4-4-6-1 以直接進樣經GC-FPD分析 146
4-4-6-2 以MA-HS-SPME萃取經GC-FPD分析 150
4-4-7微波頂空固相微萃取與液液相/固相萃取方法比較 150
4-5 水中170種農藥分析之研究: 154
4-5-1 氣相層析與分離管柱之選擇 154
4-5-2 固相微萃取纖維塗覆種類及厚度選擇之影響 154
4-5-3 固相微萃取纖維吸附率之探討 167
第五章 結論與未來發展方向 192
參考文獻 193
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