Saraji Mohammad, Ghani Milad
Department of Chemistry, Isfahan University of Technology, Isfahan 84156-83111, Iran.
Department of Chemistry, Isfahan University of Technology, Isfahan 84156-83111, Iran.
J Chromatogr A. 2015 Oct 30;1418:45-53. doi: 10.1016/j.chroma.2015.09.062. Epub 2015 Sep 25.
A method based on the combination of hollow fiber liquid-liquid-liquid microextraction and solid-phase microextraction (SPME) followed by gas chromatography-electron capture detection was developed for the determination of chlorophenols in water and wastewater samples. Silica microstructures fabricated on the surface of a stainless steel wire were coated by an organic solvent and used as a SPME fiber. The analytes were extracted through a hollow fiber membrane containing n-decane from sample solution to an alkaline aqueous acceptor phase. They were then extracted and in situ derivatized on the SPME fiber using acetic anhydride. Experimental parameters such as the type of extraction solvent, acceptor phase NaOH concentration, donor phase HCl concentration, the amount of derivatizing reagent, salt concentration, stirring rate and extraction time were investigated and optimized. The precision of the method for the analytes at 0.02-30μgL(-1) concentration level ranged from 7.1 to 10.2% (as intra-day relative standard deviation) and 6.4 to 9.8% (as inter-day relative standard deviation). The linear dynamic ranges were in the interval of 5-500μgL(-1), 0.05-5μgL(-1), 0.02-1μgL(-1) and 0.001-0.5μgL(-1) for 2-chlorophenol, 2,4-dichlorophenol, 2,4,6-trichlorophenol and pentachlorophenol, respectively. The enrichment factors were between 432 and 785. The limits of detection were in the range of 0.0004-1.2μgL(-1). Tap water, well water and wastewater samples were also analyzed to evaluate the method capability for real sample analysis.
开发了一种基于中空纤维液-液-液微萃取与固相微萃取（SPME）相结合，随后进行气相色谱-电子捕获检测的方法，用于测定水和废水样品中的氯酚。在不锈钢丝表面制备的二氧化硅微结构用有机溶剂进行涂覆，并用作SPME纤维。分析物通过含有正癸烷的中空纤维膜从样品溶液中萃取到碱性水接受相中。然后，它们在SPME纤维上使用乙酸酐进行萃取和原位衍生化。研究并优化了萃取溶剂类型、接受相氢氧化钠浓度、供体相盐酸浓度、衍生化试剂用量、盐浓度、搅拌速率和萃取时间等实验参数。该方法对浓度在0.02 - 30μg L⁻¹水平的分析物的精密度范围为7.1%至10.2%（日内相对标准偏差）和6.4%至9.8%（日间相对标准偏差）。2-氯酚、2,4-二氯酚、2,4,6-三氯酚和五氯酚的线性动态范围分别为5 - 500μg L⁻¹、0.05 - 5μg L⁻¹、0.02 - 1μg L⁻¹和0.001 - 0.5μg L⁻¹。富集因子在432至785之间。检测限在0.0004 - 1.2μg L⁻¹范围内。还对自来水、井水和废水样品进行了分析，以评估该方法对实际样品分析的能力。
