Department of Chemistry, Lanzhou University, Lanzhou, 730000 PR China.
Talanta. 2010 Mar 15;80(5):1619-25. doi: 10.1016/j.talanta.2009.09.047. Epub 2009 Oct 3.
In this paper, a rapid and sensitive method for the determination of ammonia and 22 aliphatic amines derivatized was established by cyclodextrin (CD) modified micellar electrokinetic chromatography with laser-induced fluorescence detection using 4-chloro-7-nitrobenzo-2-oxa-1,3-diazole as a derived reagent. By a series of unvaried studies, the best conditions were selected using 20mM tetraborate (pH 9.70) containing 25 mM SDS, 7 mM beta-CD, 10% acetonitrile, 0.5M urea, and applied voltage 25 kV. Under the optimum conditions, ammonia and 22 aliphatic amines were separated successfully in 19 min. The signal response was linear over three-order of concentrations. The intra-day and inter-day relative standard deviations (RSD) were less than 0.81% and 1.00% for migration times, 1.76% and 2.01% for peak areas. Limits of detection (LOD) for the analytes was (S/N=3) approximate 10(-9)-10(-12)M. The method was applied to the determination of ammonia and aliphatic amines in environmental water with recoveries in the range of 90.2-110.8%. In addition, a quantitative structure-property relationship (QSPR) model for the estimation of the electrophoretic migration time was established with the comprehensive descriptors for structural and statistical analysis (CODESSA) program for the first time. The multilinear regression (MLR) equation contained two theoretical descriptors and had the following statistical indices: R(2)=0.9668, F=290.7839, R(cv)(2)=0.9576 and S(2)=0.8149.
本文建立了一种快速灵敏的方法,通过环糊精(CD)修饰的胶束电动色谱与激光诱导荧光检测,用 4-氯-7-硝基苯并-2-氧杂-1,3-二唑作为衍生试剂,测定氨和 22 种脂肪胺。通过一系列不变的研究,选择了最佳条件,即在 20mM 四硼酸盐(pH 9.70)中含有 25mM SDS、7mMβ-CD、10%乙腈、0.5M 尿素和 25kV 的应用电压。在最佳条件下,氨和 22 种脂肪胺在 19 分钟内成功分离。信号响应在三个浓度范围内呈线性。日内和日间迁移时间的相对标准偏差(RSD)小于 0.81%和 1.00%,峰面积的相对标准偏差(RSD)小于 1.76%和 2.01%。分析物的检测限(LOD)(S/N=3)约为 10(-9)-10(-12)M。该方法应用于环境水中氨和脂肪胺的测定,回收率在 90.2-110.8%之间。此外,首次利用综合描述符(CODESSA)程序,建立了用于估算电泳迁移时间的定量结构-性质关系(QSPR)模型。多元线性回归(MLR)方程包含两个理论描述符,具有以下统计指标:R(2)=0.9668,F=290.7839,R(cv)(2)=0.9576 和 S(2)=0.8149。