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    高師機構典藏 NKNUIR > 理學院 > 化學系 > 博碩士論文 >  Item 987654321/17488
    Please use this identifier to cite or link to this item: http://ir.nknu.edu.tw/ir/handle/987654321/17488


    題名: 微波輔助頂空溫控固相微萃取技術結合氣相層析質譜儀檢測水樣品中合成除蟲菊類農藥殘留之研究
    Microwave-assisted headspace temperature-controlled solid phase microextraction combined with gas chromatography-mass spectrometry for determination of pyrethroids
    Authors: 黃靖文
    Jing-Wun Huang
    貢獻者: 徐永源;張玉珍
    Youn-Yuen Shu;Yu-Jan Chang
    Keywords: 微波;固相微萃取;合成除蟲菊類;氣相層析質譜儀
    Date: 2012-07-24
    Issue Date: 2012-11-26 10:06:37 (UTC+8)
    Abstract: 本研究是開發一個快速且靈敏的方法,微波輔助頂空溫控固相微萃取技術結合氣相層析化學游離負離子質譜術檢測水樣品中微量的合成除蟲菊類農藥。微波輔助頂空固相微萃取技術結合頂空冷凝系統進行分析物萃取的前處理/濃縮方式以促進固相微萃取對於除蟲菊類農藥的萃取效率,並以探討微波的功率、冷凝的溫度、萃取的時間、磁石的轉速、鹽類的添加、酸鹼值等可能影響之因素,尋求適當的萃取條件;以PDMS微萃取相在微波瓦數為250W、上部空間冷凝溫度為15℃、磁石轉速為800 rpm、氯化鈉濃度0.5M、pH值為4,萃取時間30分鐘,萃取後將fiber於氣相層析質譜儀中脫附5分鐘,此方法所得到的線性範圍在50~5000 ng/L之間所得之,線性相關係數R2介於0.9932~0.9996之間,偵測極限介於2.7~24.6 ng/L。實驗結果顯示微波輔助暨冷凝系統頂空固相微萃取結合氣相層析質譜儀可有效偵測真實水樣品包含河水、茶葉中微量合成除蟲菊脂類化合物,此方法有助於提高低揮發性物質的靈敏度與選擇性。
    The pretreatment technique of microwave-assisted headspace developed and studied for the extraction of pyrethroids in aqueous samples prior to the chromatographic analysis .The optimum conditions for obtaining extraction efficiency, such as the microwave power, headspace temperature, extraction time, stirring rate, pH value, and addition of salts parameters were investigated .The detection limit of the developed method is better than the conventional technique .Real samples were analyzed using the optimized condition with acceptable reproducibility.
    Experimental results indicated that the proposed MA-HSTC-SPME technique attained the best extraction efficiency under the optimized conditions, i.e.,under 220W microwave power for 30 min . The detection was linear at 50 pg/mL ~ 5000 pg/mL with correlation coefficient exceeded 0.9932 .The detection limit obtained were between 2.7 to 24.6 pg/mL, The relative standard deviation range were between 0.4 to 12.1 %(n=3) . Real samples collected from market and its own cook .
    Appears in Collections:[化學系] 博碩士論文
    [化學系] 徐永源
    [化學系] 張玉珍

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