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標題: 吹氣輔助頂空固相微萃取結合氣相層析質譜術於水中硝基多環芳香烴之研究
Purge Assisted Headspace Solid Phase Microextraction Combined with Gas Chromatography/Mass Spectrometry for Determination of Nitrated Polycyclic Aromatic Hydrocarbons in Aqueous Solution
作者: 洪晟瀚
Hung, Cheng-Han
關鍵字: 吹氣輔助頂空固相微萃取;Purge Assisted Headspace Solid Phase Microextraction;氣相層析質譜術;硝基多環芳香烴;環境分析;Gas Chromatography/Mass Spectrometry;Nitrated Polycyclic Aromatic Hydrocarbons;Environmental analysis
出版社: 化學系所
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實驗結果顯示以吹氣輔助頂空固相微萃取結合氣相層析質譜術,以負離子化學游離化法選擇離子偵測模式,進行水中微量硝基多環芳香烴化合物之研究,於10 mL水樣品中,添加pH值為4.5的緩衝溶液與25 %的NaCl,於氮氣流速30 mL/min下,以100 μm PDMS固相微萃取塗覆纖維於90 °C水浴下,萃取45分鐘,再於氣相層析儀的程序升溫注射口下脫附7.5分鐘,所測得水中硝基多環芳香烴的線性範圍為5 – 5000 pg/mL,其線性相關係數介於0.996至0.999,偵測極限則介於0.01 - 0.11 pg/mL之間。此方法也應用於真實河川樣品之分析。結果顯示以吹氣輔助頂空固相微萃取結合氣相層析質譜儀可大幅提升低揮發性物質之靈敏度與選擇性,可做為水樣品中微量硝基多環芳香烴化合物檢測之參考。

This study was evaluated to determine trace seven nitrated polycyclic aromatic hydrocarbons (NPAHs) in aqueous solution by using purge assisted headspace solid phase microextraction (PA-HS-SPME) combined with gas chromatography/mass spectrometry in negative ion chemical ionization (GC/NICI-MS). The proposed method was based on continuous purging gas through the sample to carry analytes to headspace in which a SPME fiber was used as sorptive device. The parameters affecting the extract efficiency such as SPME fiber, extraction temperature, extraction time, agitation rate, salt effect, pH, hollow fiber length, and nitrogen flow rate were systematically studied. Compared to HS-SPME, PA-HS-SPME provides a significantly improved sensitivity for the extraction of NPAHs, especially for less-volatile NPAHs which could not be detected by HS-SPME. The linear range was 5 - 5000 pg/mL with correlation coefficients above 0.996. Limits of detection (LOD) of seven NPAHs were in the range of 0.01 to 0.10 pg/mL. The application of the methods to the determination of NPAHs in real samples was tested by analyzing aqueous samples from rivers in Taichung city.
其他識別: U0005-2008200811252300
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