Hsieh Yi-Chien, Whang Chen-Wen
Department of Chemistry, Tunghai University, Taichung 407, Taiwan.
J Chromatogr A. 2006 Jul 28;1122(1-2):279-82. doi: 10.1016/j.chroma.2006.05.078. Epub 2006 Jun 22.
A capillary electrophoresis (CE) coupled with electrochemiluminescence (ECL) detection method for the analysis of ethambutol (EB) and methoxyphenamine (MP) has been investigated. Complete separation of EB and MP was achieved in 8 min using a background electrolyte of 20 mM sodium phosphate at pH 10.0 and a separation voltage of 9 kV. ECL detection was performed with an indium/tin oxide (ITO) working electrode biased at 1.4 V (versus a Pt wire reference) in a 200 mM sodium phosphate buffer (pH 8.0) containing 3.5 mM Ru(bpy)3(2+) (where bpy = 2,2'-bipyridyl). Linear correlation (r > or = 0.993) between ECL intensity and drug concentration was obtained in the range 2-50 ng/ml. The limits of detection (LODs) for EB and MP in water were 1.0 and 0.9 ng/ml, respectively. The relative standard deviation values on peak size (10 ng/ml level) and migration time for the two drugs were in the ranges 5-8 and 0.2-0.7% (n = 7), respectively. Applicability of the CE-ECL method to the analysis of human plasma spiked with EB and MP was examined. The LODs for EB and MP in plasma were 0.4 and 0.3 microg/ml, respectively.
研究了一种用于分析乙胺丁醇(EB)和甲氧那明(MP)的毛细管电泳(CE)与电化学发光(ECL)检测联用的方法。使用pH值为10.0的20 mM磷酸钠作为背景电解质,分离电压为9 kV,在8分钟内实现了EB和MP的完全分离。在含有3.5 mM Ru(bpy)3(2+)(其中bpy = 2,2'-联吡啶)的200 mM磷酸钠缓冲液(pH 8.0)中,以偏置在1.4 V(相对于铂丝参比电极)的氧化铟锡(ITO)工作电极进行ECL检测。在2 - 50 ng/ml范围内获得了ECL强度与药物浓度之间的线性相关性(r≥0.993)。水中EB和MP的检测限(LOD)分别为1.0和0.9 ng/ml。两种药物在10 ng/ml水平下峰面积和迁移时间的相对标准偏差值分别在5 - 8%和0.2 - 0.7%范围内(n = 7)。考察了CE - ECL方法用于分析加有EB和MP的人血浆的适用性。血浆中EB和MP的LOD分别为0.4和0.3 μg/ml。