Lou Da-Wei, Lee Xinqing, Pawliszyn Janusz
Department of Chemistry, University of Waterloo, Waterloo, Ontario N2L 3G1, Canada; Department of Chemistry, Jilin Institute of Chemical Technology, Jilin, Jilin 132022, China.
J Chromatogr A. 2008 Aug 8;1201(2):228-34. doi: 10.1016/j.chroma.2008.02.066. Epub 2008 Feb 23.
A combined method of dynamic headspace-needle trap sample preparation and gas chromatography for the determination of formic and acetic acids in aqueous solution was developed in this study. A needle extraction device coupled with a gas aspirating pump was intended to perform sampling and preconcentration of target compounds from aqueous sample before gas chromatographic analysis. The needle trap extraction (NTE) technique allows for the successful sampling of short chain fatty acids under dynamic conditions while keeping the headspace (HS) volume constant. Two important parameters, including extraction temperature and effect of acidification, have been optimized and evaluated using the needle trap device. The method detection limits for the compounds estimated were 87.2microg/L for acetic acid and 234.8microg/L for formic acid in spite of the low flame ionization detection response for formic acid and its low Henry's law constant in aqueous solution. Precision was determined based on the two real samples and ranged between 4.7 and 10.7%. The validated headspace-needle trap extraction method was also successfully applied to several environmental samples.
本研究开发了一种动态顶空-针捕集样品制备与气相色谱联用的方法,用于测定水溶液中的甲酸和乙酸。一种与气体抽吸泵相连的针式萃取装置,旨在对水样中的目标化合物进行采样和预浓缩,然后进行气相色谱分析。针捕集萃取(NTE)技术能够在动态条件下成功采集短链脂肪酸,同时保持顶空(HS)体积恒定。利用针捕集装置对两个重要参数,即萃取温度和酸化效果进行了优化和评估。尽管甲酸在火焰离子化检测中的响应较低,且在水溶液中的亨利定律常数也较低,但所测化合物的方法检出限分别为:乙酸87.2μg/L,甲酸234.8μg/L。基于两个实际样品测定的精密度在4.7%至10.7%之间。经验证的顶空-针捕集萃取方法也成功应用于多个环境样品。