開發頂空中空纖維液相微萃取合併氣相層析-質譜儀測量水樣或血清中揮發性有機物

Development of headspace hollow fiber liquid-phase microextraction to identify volatile organic compounds in aqueous sample or serum using gas chromatography-mass spectrometry

曾昱翔(Yu-Hsiang Tseng)

指導教授 ： 陳珮珊

國立臺灣大學/醫學院/法醫學研究所/碩士(2014年)

https://doi.org/10.6342/NTU.2014.03056

摘要

本實驗開發中空纖維輔助的頂空液相微萃取法(HS-HF-LPME)搭配氣相層析質譜儀偵測水樣或血清中的七種揮發性有機物(VOCs)。本方法藉由圓環狀的中空纖維的幫助，萃取溶劑在萃取過程中不會有掉落的危險，並以不含鹵素的正辛醇做為萃取溶劑，單次萃取用量為23 μL，使用量低於傳統的液相萃取，對環境較為友善。
方法最佳化的實驗在水樣中進行，在加熱器設定95°C萃取20分鐘的最佳化的條件下，濃縮倍數介於9 – 69倍，線性在0.9957-0.9999，偵測極限約為2.6 – 46.4 ng mL-1，再現性的標準偏差在13.3%以下。萃取血清檢體得到的相對回收率為44 – 100.1%，絕對回收率在5.8 – 45.6%，其中甲苯及二甲苯的相對回收率受到明顯的基質效應影響。
本方法的萃取過程步驟少、溶劑的用量小、利用簡單的實驗器材、再現性佳，是個簡單且環保的萃取方法，但較不適合用於基質複雜的血清或血液檢體。

關鍵字

頂空液相微萃取 ； 中空纖維輔助液相微萃取 ； 揮發性有機物 ； 氣相層析質譜儀

並列摘要

The sample preparation method in this study “Overhand knot hollow fiber-assisted headspace liquid-phase microextraction” (OK-HF-HS-LPME) coupled with gas chromatography-mass spectrometry has been developed for the analysis of seven volatile organic compounds (VOCs) in aqueous sample or serum. A loose overhand knot tied by hollow fiber was hung in the headspace for extraction. As the shape of knot was easy to hold more extraction solvent (23 μL), large volume of extraction solvent lasts longer extraction time (20 min) and higher extraction temperature. This improves the extraction of headspace significantly.
Under the optimized condition, 7 VOCs (diethyl ether, ethyl acetate, dichloromethane, toluene, p-xylene, m-xylene, o-xylene) in spiked D.I. water, 23 μL octanol was used for extraction. After the 20 min at high heating temperature of 95°C, there was still enough solvent (more than 7 μL) remained for GC analysis. The linear range of the method was 0.1-80 μg mL-1 for 3 VOCs (diethyl ether, ethyl acetate, dichloromethane) and 0.01-8 μg mL-1 for the other 4 VOCs (toluene, p-xylene, m-xylene, o-xylene). The limit of detection was in the range of 0.0026-0.0464 μg mL-1. Enrichment factors ranged from 9 to 69 folds.
The optimized extraction parameters were used for the extraction of 7 VOCs in spiked serum. The relative recovery ranged from 43.6% to 100.1%. It showed that the extraction efficiency of some analytes (toluene, p-xylene, m-xylene, o-xylene) was affected by the matrix of serum.
The study is a simple, low-cost and environmental-friendly sample preparation technique, but it needs carefully manual manipulation to achieve good precision. In the application of real sample, this method is more suitable for the extraction of aqueous sample than matrix-complex serum or blood.

並列關鍵字

HS-LPME ； Hollow fiber LPME ； VOCs ； GC-MS

參考文獻

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