García-Valverde M T, Lucena R, Cárdenas S, Valcárcel M
Department of Analytical Chemistry, Institute of Fine Chemistry and Nanochemistry, Marie Curie Building, Campus of Rabanales, University of Córdoba, 14071 Córdoba, Spain.
Department of Analytical Chemistry, Institute of Fine Chemistry and Nanochemistry, Marie Curie Building, Campus of Rabanales, University of Córdoba, 14071 Córdoba, Spain.
J Chromatogr A. 2016 Sep 16;1464:42-9. doi: 10.1016/j.chroma.2016.08.036. Epub 2016 Aug 16.
In this article, carbon fibres (CFs) are presented as sorbent material for the dispersive micro-solid phase extraction of twelve chlorophenols from urine samples. CFs are synthesized by a reagentless and green procedure consisting of heating raw cotton, a natural precursor, at high temperature (400°C) in an inert atmosphere (Ar) during 2h. The resulting fibres, which present good water dispersibility, are finally loaded on an in-syringe device. This device, which integrates the extraction and final elution of the analytes, is disposable and it is adapted to process low sample volumes. Working at the optimum conditions, the extraction procedure in combination with gas chromatography/mass spectrometry allows the determination of the analytes in urine at the low μg/L range. In fact, the limits of quantification (LOQs) of the analytes were in the interval from 1μg/L to 2.5μg/L with precision values, expressed as relative standard deviations (RSD), better than 13%. Relative recovery values, ranging from 74.5% to 113%, demonstrate the applicability of the proposed method.
在本文中，碳纤维（CFs）被用作吸附剂材料，用于从尿液样本中分散微固相萃取十二种氯酚。碳纤维通过一种无试剂的绿色方法合成，该方法包括在惰性气氛（氩气）中于400°C高温下加热天然前驱体生棉2小时。所得纤维具有良好的水分散性，最终被加载到注射器装置上。该装置集成了分析物的萃取和最终洗脱，是一次性的，适用于处理少量样品。在最佳条件下工作时，萃取程序与气相色谱/质谱联用可测定尿液中低μg/L范围内的分析物。事实上，分析物的定量限（LOQs）在1μg/L至2.5μg/L之间，以相对标准偏差（RSD）表示的精密度值优于13%。相对回收率在74.5%至113%之间，证明了该方法的适用性。
