臺灣博碩士論文加值系統

本研究為開發水浴頂空固相微萃取(Water-bath headspace solid-phase microextraction，WB-HSSPME)、水浴頂空磁轉子吸附萃取(Water-bath headspace stir bar sorptive extraction，WB-HSSBSE)、微波輔助頂空固相微萃取(Microwave-assisted headspace solid-phase microextraction，MA-HSSPME)、微波輔助頂空磁轉子吸附萃取(Microwave assisted headspace stir bar sorptive extraction，MA-HSSBSE)，分析飲用水中所含的臭味化合物2-Methylisoborneol (2-MIB)與Geosmin (GSM)，研究中探討萃取時間、萃取溫度、加鹽比例效應、頂空-樣品接觸面積、吸附材料（PDMS、PDMS-DVB）等可能影響的因素，結果發現以PDMS-DVB萃取效果最好，其最佳化條件為：WB-HSSPME在75℃、25％的NaCl、萃取75分鐘可得最高的回收率；MD-HSSPME在75℃、20％NaCl、萃取75分鐘可得最高回收率。檢量線的線性範圍為0.5 ng/L到250 ng/L，其R2 > 0.99，上述分析方法用於飲用水源經淨水廠處理後的水棟樣品分析

Headspace sorptive techniques namely water-bath headspace solid-phase microextraction (WB-HSSPME), microwave-assisted headspace solid-phase microextraction (MA-HSSPME), water-bath headspace stir bar sorptive extraction (WB-HSSBSE), microwave-assisted headspace stir bar sorptive extraction (MA-HSSBSE) were developed and studied for the simultaneous extraction/enrichment of ordor compounds, 2-methylisoborneol (2-MIB) and geosmin(GSM), in the drinking water samples prior to the quantification by gas chromatograph-mass spectrometer (GC-MS). The odor compounds in aqueous media were extracted onto a solid-phase micro fibre or stir bar sorptive material via the headspace with the aid of microwave-assisted or water-bath heating. The optimum conditions for obtaining extraction efficiency, such as extraction time, extraction temperature, addition of salt, sorbent material, and the desorption parameters were investigated. Experimental results indicat that the optimized MA-HSSPME technique is 75min at 75℃ with 25 % NaCl addition to give 20.1% and 53.1 % recoveries of 2-MIB and GSM, respectively; whereas the optimized WB-HSSPME technique is 75min at 75℃ with 20 % NaCl addition to give 17.4 % and 61.36 % recoveries of 2-MIB and GSM, respectively. The interface area between aqueous and gas phases did not provide significant difference in the extraction efficiency. The correlation coefficients for the linear dynamic range from 0.5 to 250 ng/l exceeded 0.99 for the both techniques. Samples collected from drinking water treatment plant were also determined by the proposed methods

第一章、緒論 1
I -1 前言 1
I -2 微波 3
I -2-1 微波發展簡介 3
I -2-2 微波加熱原理與萃取機制 5
I -2-3 影響微波的因素 13
I -2-4 微波加熱與傳統加熱的比較 15
I -2-5 本實驗微波萃取裝置 16
I -3 固相微萃取 19
I -3-1 固相微萃取發展簡介 19
I -3-2 固相微萃取與頂空固相微萃取的原理 23
I -3-3 固相微萃取的優點 27
I -4 磁轉子吸附萃取裝置 27
I -5 氣相層析質譜儀(Gas Chromatography-Mass Spectrometry，GC-MS) 29
I -6 分析化合物2-MIB與GSM的方法 30
I -7 研究目的 33
第二章、實驗 36
II -1 實驗流程 36
II -2 藥品與試劑 36
II -2-1 溶劑 36
II -2-2 標準品 37
II -2-3 內標準品 37
II -2-4 標準水溶液 37
II -2-5 檢量標準水溶液 37
II -2-6 內標物水溶液 38
II -3 實驗儀器設備 38
II -3-1 萃取用玻璃瓶 39
II -4 分析儀器 41
II -4-1 氣相層析質譜儀 ( GC-MS，HP5890-5971) 41
II -4-2 熱脫附系統氣相層析質譜儀(TDS2-CIS4-GC-MS，HP6890-5973) 41
II -4-3 氣相層析質譜儀選擇離子監測模式(Select Ion Monitor Mode，SIM) 42
II -5 萃取纖維的活化 43
II -5-1 萃取裝置的活化 ( Conditioning or Activation ) 43
II -6 水浴加熱固相微萃取纖維與磁轉子吸附萃取最佳化條件的探討 44
II -6-1 萃取時間對分析物回收率的影響 44
II -6-2 萃取溫度對分析物回收率的影響 44
II -6-3 加鹽比例對分析物回收率的影響 44
II -6-4 頂空與樣品接觸面積對分析物回收率的影響 45
II -6-5 固相微萃取塗附靜相對分析物回收率的影響 45
II -6-6 水浴加熱的檢量線 46
II -7 微波輔助固相微萃取纖維與磁轉子吸附萃取最佳化條件的探討 46
II -7-1 萃取時間對分析物回收率的影響 46
II -7-2 萃取溫度對分析物回收率的影響 47
II -7-3 加鹽比例對分析物回收率的影響 47
II -7-4 頂空與樣品接觸回收率對分析物回收率的影響 47
II -7-5 固相微萃取塗附靜相對分析物回收率的影響 48
II -7-6 微波加熱的檢量線 48
II -8 真實樣品的檢測 48
第三章、結果與討論 50
III -1 直接注射法分析2-MIB與Geosmin標準溶液與內標物Borneol標準溶液氣相層析圖與質譜圖 50
III -2 水浴加熱頂空固相微萃取纖維與頂空磁轉子吸附萃取氣相層析圖 50
III -3 微波輔助頂空固相微萃取纖維與頂空磁轉子吸附萃取氣相層析圖 51
III -4 水浴加熱頂空固相微萃取纖維與頂空磁轉子吸附萃取最佳化條件的探討 56
III -4-1 水浴萃取時間對分析物回收率的影響 56
III -4-2 水浴萃取溫度對分析物回收率的影響 56
III -4-3 加鹽比例對分析物回收率的影響 57
III -4-4 頂空與樣品接觸面積對分析物回收率的影響 58
III -4-5 固相微萃取塗附靜相對分析物回收率的影響 58
III -5 微波輔助頂空固相微萃取纖維與頂空磁轉子吸附萃取最佳化條件的探討 69
III -5-1 萃取時間對分析物回收率的影響 69
III -5-2 萃取溫度對分析物回收率的影響 69
III -5-3 加鹽比例對分析物回收率的影響 70
III -5-4 頂空與樣品接觸面積對分析物回收率的影響 70
III -5-5 頂空固相微萃取塗附靜相對分析物回收率的影響 71
III -6 檢量線與偵測極限 81
III -6-1 水浴加熱頂空固相微萃取的檢量線與偵測極限 81
III -6-2 微波輔助頂空固相微萃取的檢量線與偵測極限 83
III -7 真實樣品檢測 84
第四章、結論 87
第五章、參考文獻 88

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