Moliner-Martínez Y, Herráez-Hernández R, Campíns-Falcó P
Departament de Química Analítica, Facultat de Química, Universitat de Valencia, C/Dr Moliner 50, E46100-Burjassot, Valencia, Spain.
J Chromatogr A. 2007 Sep 14;1164(1-2):329-33. doi: 10.1016/j.chroma.2007.07.066. Epub 2007 Aug 1.
A new microscale method is presented for the determination of ammonium and primary short-chain aliphatic amines (methylamine, ethylamine, propylamine, n-butylamine and n-pentylamine) in water. The assay uses precolumn derivatization with the reagent o-phthaldialdehyde (OPA) in combination with the thiol N-acetyl-L-cysteine (NAC), and capillary liquid chromatography with UV detection at 330 nm. The described method is very simple and rapid as no preconcentration of the analytes is necessary, and the volume of sample required is only 0.1 mL. Under the proposed conditions good linearity has been obtained up to a concentration of the analytes of 10.0 mgL(-1), the limits of detection being of 8-50 microgL(-1). No matrix effect was found, and recoveries between 97 and 110% were obtained. The precision of the method was good, and the achieved variation coefficients were below 12%. The reliability of the proposed approach has been tested by analyzing a microsample of fogwater collected from leaf surfaces.
本文提出了一种用于测定水中铵和主要短链脂肪胺（甲胺、乙胺、丙胺、正丁胺和正戊胺）的新的微量分析方法。该分析方法采用邻苯二甲醛（OPA）试剂与硫醇N-乙酰-L-半胱氨酸（NAC）进行柱前衍生化，并结合在330 nm处进行紫外检测的毛细管液相色谱法。所描述的方法非常简单快速，因为无需对分析物进行预浓缩，所需样品体积仅为0.1 mL。在所提出的条件下，分析物浓度高达10.0 mgL(-1)时获得了良好的线性，检测限为8-50 microgL(-1)。未发现基质效应，回收率在97%至110%之间。该方法的精密度良好，变异系数低于12%。通过分析从叶片表面收集的雾水微量样品，测试了所提出方法的可靠性。
