Lloret S Meseguer, Andrés J Verdú, Legua C Molins, Falcó P Campíns
Department of Analytical Chemistry, University of Valencia, Dr. Moliner 50, 46100-Burjassot, Valencia, Spain.
Talanta. 2005 Feb 28;65(4):869-75. doi: 10.1016/j.talanta.2004.08.050.
A method for the simultaneous determination of primary amino groups and ammonium ion has been proposed. The method is based in solution derivatization with o-Phthaldialdehyde/N-acetyl-cisteine (OPA/NAC) and fluorescence measurement of the formed isoindols. Analytical characteristics and description of the developed procedure have been provided. The calibration graphs for ammonium (up to 1.44mgL(-1) of N) and methylamine as primary amino model compound (up to 0.282mgL(-1) of N), were obtained. Bivariate and multivariate calibration models have been tested. The limits of detection were 0.07mgL(-1) of N and 0.004mgL(-1) of N for ammonium and amine, respectively. The procedure was first applied directly to standard solutions containing ammonium and amines and secondly to digested solutions by Kjeldahl method. The results obtained allowed to establish the best digestion conditions in order to perform the total amine conversion into ammonium. This procedure has been also applied to real samples (irrigation ditch, residual and fountain waters) and the concentrations of primary amine groups and ammonium have been evaluated. The results obtained after Kjeldahl digestion allowed to estimate the total Kjeldahl N contained in the samples. The samples were also analysed by Nessler method and similar results were obtained.
提出了一种同时测定伯氨基和铵离子的方法。该方法基于邻苯二甲醛/N-乙酰半胱氨酸(OPA/NAC)的溶液衍生化以及对形成的异吲哚进行荧光测量。提供了所开发方法的分析特性和描述。获得了铵(高达1.44mgL(-1)的N)和作为伯氨基模型化合物的甲胺(高达0.282mgL(-1)的N)的校准曲线。测试了双变量和多变量校准模型。铵和胺的检测限分别为0.07mgL(-1)的N和0.004mgL(-1)的N。该方法首先直接应用于含有铵和胺的标准溶液,其次应用于凯氏定氮法消化后的溶液。所获得的结果有助于确定最佳消化条件,以便将总胺转化为铵。该方法也已应用于实际样品(灌溉沟渠水、残留水和喷泉用水),并评估了伯胺基团和铵的浓度。凯氏定氮消化后获得的结果有助于估计样品中总凯氏氮的含量。样品也用奈斯勒法进行了分析,获得了相似的结果。