Department of Analytical Chemistry, Institute of Fine Chemistry and Nanochemistry, Marie Curie Building, Campus de Rabanales, University of Córdoba, 14071 Córdoba, Spain.
J Chromatogr A. 2012 Mar 16;1229:48-54. doi: 10.1016/j.chroma.2012.01.026. Epub 2012 Jan 18.
A simple and efficient method for the determination of ten chlorophenols (including mono, di, tri, tetra and pentachlorophenols) in water samples is presented. The analytical method is based on a previous derivatization of the target compounds with acetic anhydride, being the derivatized compounds finally isolated/preconcentrated by an in situ solvent formation microextraction. Later on the extractant (an ionic liquid) containing the analytes is recovered by centrifugation and thermally desorbed. The analytes are finally separated and determined by gas chromatography/mass spectrometry. The main variables involved in the extraction and thermal desorption steps have been studied in depth. Once evaluated, the analytical method has been characterized in terms of linearity, sensitivity, precision and accuracy. The limits of detection were in the range from 60 ng L(-1) (4-chlorophenol) to 440 ng L(-1) (pentachlorophenol) while the precision, expressed as relative standard deviation, was in the interval from 4.5% (2,6-dichlorophenol) to 9.9% (3-chlorophenol). In addition, acceptable recovery values were obtained in samples of different nature, including river, tap and reservoir water samples.
本文提出了一种测定水样中十种氯苯酚（包括单氯、二氯、三氯、四氯和五氯苯酚）的简单高效方法。该分析方法基于目标化合物与乙酸酐的衍生化，衍生化产物最终通过原位溶剂形成微萃取进行分离/预浓缩。然后，通过离心回收含有分析物的萃取剂（离子液体），并进行热解吸。最后，通过气相色谱/质谱法对分析物进行分离和测定。深入研究了萃取和热解吸步骤中涉及的主要变量。在评估后，该分析方法在线性度、灵敏度、精密度和准确度方面进行了表征。检测限范围为 60ng/L（4-氯苯酚）至 440ng/L（五氯苯酚），而精密度（表示为相对标准偏差）在 4.5%（2,6-二氯苯酚）至 9.9%（3-氯苯酚）之间。此外，在不同性质的样品中，包括河水、自来水和水库水样中，均获得了可接受的回收率值。
