Teich Monique, van Pinxteren Dominik, Herrmann Hartmut
Chemistry Department, Leibniz-Institut für Troposphärenforschung (TROPOS), Leipzig, Germany.
Electrophoresis. 2014 May;35(9):1353-61. doi: 10.1002/elps.201300448. Epub 2014 Jan 29.
A hollow-fiber liquid-phase microextraction method was developed to enrich nine nitrophenolic compounds from aqueous extracts of atmospheric aerosol particles. Analysis was performed by CE coupled with ESI MS. The BGE composition was optimized to a 20 mM ammonium acetate buffer at pH 9.7 containing 15% methanol v/v. Several extraction parameters (composition of organic liquid membrane, pH of acceptor phase, salting-out effect, extraction time) were investigated for their effect on the analyte recoveries. The donor phase consisted of a 1.8 mL sample solution kept at pH 2 while the acceptor phase was a 15 μL 100 mM aqueous ammonia solution. Dihexyl ether served as supported liquid membrane. Low detection limits in the range of nanomole per liter were achieved. Recoveries of aqueous standard solutions were found to be between 11 and 90% with enrichment factors between 10 and 100. Interday and intraday repeatabilities were in an acceptable range for most compounds (6-15% and 7-10%, respectively) but somewhat higher for 4-nitrocatechol (59 and 48%) and 2-nitrophenol (17 and 35%). The developed method was found to be competitive with more established method and was successfully applied to samples of atmospheric particulate matter from field experiments.
开发了一种中空纤维液相微萃取方法,用于从大气气溶胶颗粒的水提取物中富集9种硝基酚类化合物。采用毛细管电泳-电喷雾电离质谱联用进行分析。将背景电解质(BGE)组成优化为pH 9.7的20 mM醋酸铵缓冲液,含15%(v/v)甲醇。研究了几个萃取参数(有机液膜组成、接收相pH值、盐析效应、萃取时间)对分析物回收率的影响。供体相为1.8 mL pH值保持在2的样品溶液,接收相为15 μL 100 mM氨水溶液。二己醚用作支撑液膜。实现了纳摩尔/升范围内的低检测限。发现水标准溶液的回收率在11%至90%之间,富集因子在10至100之间。大多数化合物的日间和日内重复性在可接受范围内(分别为6-15%和7-10%),但4-硝基邻苯二酚(59%和48%)和2-硝基苯酚(17%和35%)稍高。发现所开发的方法与更成熟的方法具有竞争力,并成功应用于现场实验的大气颗粒物样品。