Department of Analytical Chemistry, Marie Curie Building (Annex), Campus de Rabanales, University of Cordoba, E-14071 Córdoba, Spain.
J Chromatogr A. 2011 Feb 18;1218(7):869-74. doi: 10.1016/j.chroma.2010.12.075. Epub 2010 Dec 23.
In this article, a novel liquid phase microextraction technique, called stir membrane liquid-liquid microextraction (SM-LLME), is presented. The new approach combines the advantages of liquid phase microextraction and stirring in the same unit allowing the isolation and preconcentration of the analytes in a simple and efficient way. In the construction of the unit, a polymeric membrane is employed to protect the small volume of the extractant phase. The extraction technique is characterized for the resolution of a model analytical problem: the determination of five selected chlorophenols in water. A two-phase extraction mode is used for the extraction of the analytes with an organic solvent in which an in situ derivatization reaction takes place. The analytes are finally analyzed by gas chromatography/mass spectrometry. All the variables involved in the extraction process have been clearly identified and optimized. The new extraction mode allows the determination of chlorophenols with limits of detection in the range from 14.8 ng/L (for 2,4,5-trichlorophenol) to 22.9 ng/L (for 3-chlorophenol) with a relative standard deviation lower than 8.7% (for 2,6-dichlorophenol).
本文提出了一种新颖的液相微萃取技术,称为搅拌膜液-液微萃取(SM-LLME)。该新方法结合了液相微萃取和搅拌的优点,在同一单元中允许以简单有效的方式分离和浓缩分析物。在单元的构建中,采用聚合物膜来保护小体积的萃取相。该萃取技术的特点是用于解决一个模型分析问题:水中五种选定的氯苯酚的测定。采用有机溶剂进行两相萃取模式,其中发生原位衍生反应。最后通过气相色谱/质谱法分析分析物。萃取过程中涉及的所有变量都已被明确识别并进行了优化。这种新的萃取模式允许用检测限在 14.8ng/L(2,4,5-三氯苯酚)至 22.9ng/L(3-氯苯酚)范围内测定氯苯酚,相对标准偏差低于 8.7%(2,6-二氯苯酚)。