Development of headspace hollow fiber liquid-phase microextraction to identify volatile organic compounds in aqueous sample or serum using gas chromatography-mass spectrometry
Date Issued
2014
Date
2014
Author(s)
Tseng, Yu-Hsiang
Abstract
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.
Subjects
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
Type
thesis
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