Department of Analytical Chemistry, Faculty of Chemistry, University of Tabriz, Tabriz, Iran.
Anal Chim Acta. 2013 May 2;775:50-7. doi: 10.1016/j.aca.2013.03.004. Epub 2013 Mar 13.
The paper presents a new method based on simultaneous derivatization and air-assisted liquid-liquid microextraction (AALLME) for the extraction and preconcentration of some aliphatic amines prior to gas chromatography-flame ionization detection (GC-FID). Primary aliphatic amines are derivatized and extracted simultaneously by a fast reaction with butylchloroformate (derivatization agent/extraction solvent) under mild conditions. The mixture of butylchloroformate and aqueous sample solution is rapidly sucked into a 10-mL glass syringe and then is injected into a test tube with conical bottom and the procedure is repeated seven times. After centrifuging the resulted cloudy solution, the derivatized analytes in the sedimented phase are determined by GC-FID. The influence of main factors on the efficiency of derivatization/extraction procedure is studied. Under the optimal conditions, the enrichment factors (EFs) for aliphatic amines are obtained in the range of 248-360 and limits of detection (LODs) are between 0.30 and 2.6 μg L(-1). The obtained extraction recoveries ranged from 50 to 72% and the relative standard deviation (RSD) was less than 4.8% for intra-day (n=6) and inter-days (n=4) precision. The method is successfully applied to determine some aliphatic amines in environmental water samples.
本文提出了一种基于同步衍生化和空气辅助液-液微萃取（AALLME）的新方法，用于在气相色谱-火焰离子化检测（GC-FID）之前提取和预浓缩一些脂肪胺。伯脂肪胺在温和条件下与丁基氯甲酸酯（衍生化试剂/萃取溶剂）快速反应，同时进行衍生化和提取。将丁基氯甲酸酯和水样混合液快速吸入 10 mL 玻璃注射器中，然后注入底部为锥形的试管中，重复此过程七次。将得到的混浊溶液离心后，通过 GC-FID 测定沉淀相中衍生化分析物的含量。研究了主要因素对衍生化/萃取过程效率的影响。在最佳条件下，得到了脂肪胺的富集因子（EF）在 248-360 范围内，检测限（LOD）在 0.30-2.6 μg L(-1) 之间。该方法的萃取回收率在 50-72%之间，日内（n=6）和日间（n=4）精密度的相对标准偏差（RSD）小于 4.8%。该方法成功应用于环境水样中一些脂肪胺的测定。
