Sarafraz-Yazdi A, Amiri A H, Es'haghi Z
Department of Chemistry, Faculty of Sciences, Ferdowsi University of Mashhad, Iran.
Chemosphere. 2008 Mar;71(4):671-6. doi: 10.1016/j.chemosphere.2007.10.073. Epub 2008 Jan 25.
In the present work, a sample pre-treatment technique for the determination of trace concentrations of benzene, toluene, ethyl benzene and xylene (BTEX) in aqueous samples has been developed and applied to analysis of the selected analytes in environmental water samples. The extraction procedure is based on coupling polypropylene hollow-fiber liquid phase microextraction (HF-LPME) with gas chromatography by flame ionization detection (GC-FID). The effective parameters such as organic solvent, extraction time, agitation speed and salting effect were investigated. Good reproducibilities of the extraction performance were obtained, with the RSD values ranging from 2.02 to 4.61% (n=5). The method provided 41.47-128.01 fold preconcentration of the target analytes. The limits of detections for the BTEX were in the range of 0.005-03microg ml(-1). In addition, sample clean-up was achieved during LPME due to the selectivity of the hollow fiber, which prevented undesirable large molecules from being extracted. Real samples (River and waste waters) containing BTEX were examined using this method with good linearity and precision (RSDs most lower than 6.00%, n=5). All experiments were carried out at room temperature, 22+/-0.5 degrees C.
在本研究中,已开发出一种用于测定水样中痕量苯、甲苯、乙苯和二甲苯(BTEX)的样品预处理技术,并将其应用于环境水样中所选分析物的分析。萃取过程基于聚丙烯中空纤维液相微萃取(HF-LPME)与火焰离子化检测气相色谱法(GC-FID)的联用。研究了有机溶剂、萃取时间、搅拌速度和盐效应等有效参数。萃取性能具有良好的重现性,相对标准偏差(RSD)值在2.02%至4.61%之间(n = 5)。该方法对目标分析物的预富集倍数为41.47至128.01倍。BTEX的检测限在0.005至0.3μg ml⁻¹范围内。此外,由于中空纤维的选择性,在液相微萃取过程中实现了样品净化,可防止不需要的大分子被萃取。使用该方法对含有BTEX的实际样品(河水和废水)进行了检测,具有良好的线性和精密度(相对标准偏差大多低于6.00%,n = 5)。所有实验均在室温22±0.5℃下进行。