Development of high quality "capillary electrophoresis-chemiluminescence detection" system and its application to a environmental sample

采用毛细管电泳-化学发光检测器对酚类化合物进行了分析。过氧草酸盐化学发光试剂与丹磺酰氯一起用作标记试剂。考察了试剂浓度、标记方法和化学发光检测池的性能对酚类化合物检测的敏感性。测定了苯酚、2-氯苯酚、4-氯苯酚、2，4-二氯苯酚、2，6-二氯苯酚和2，4，6-三氯苯酚等6种酚类化合物，检测限为10-7 M量级，检测范围为3个数量级。比普通荧光检测器低10倍。以十二烷基硫酸钠和乙腈为运行缓冲液，对15种酚类化合物进行了分离。将毛细管、电泳-化学发光检测器和柱浓缩过程相结合，使该系统能够应用于地表水和回用沃茨等真实的样品，并利用毛细管尖端的微空间进行反应/检测，实现了多个样品的同时分析。采用1，10-邻菲咯啉与过氧化氢的化学发光反应，以Cu（II）为模型化合物。将三种不同长度的毛细管插入聚四氟乙烯管制成的流动式化学发光检测池中。三种样品同时在相应的毛细管中迁移，并在毛细管尖端与CL试剂混合产生化学发光。在本系统中的多个样品的同时分析支持的可能性，真实的样品可以更容易地确定，快速，准确的校准图。

Phenolic compounds were analyzed by means of capillary electrophoresis with chemiluminescence detector. Peroxyoxalate chemiluminescence reagent was used together with dansyl chloride as a labeling reagent. The reagent concentrations, the labeling procedures, and the performance of chemiluminescence detection cells were examined for sensitive detection of phenolic compounds. Six kinds of phenolic compounds (phenol, 2-chlorophenol, 4-chlorophenol, 2,4-dichlorophenol, 2,6-dichlorophenol, and 2,4,6-trichlorophenol) were determined over a range of 3 orders of magnitude with the detection limits of 10-7 M order; their detection limits were ca. 10 times as low as those obtained by an ordinary fluorescence detector. A running buffer solution containing SDS and acetonitrile provided satisfactory results in separation of fifteen kinds of phenolic compounds. The combination of capillary, electrophoresis with chemiluminescence detector and column concentration procedure supported the possibility that the present system could be applied to real samples such as surface and reused waters.Also, plural samples were simultaneously analyzed in the electrophoresis - chemiluminescence detector system, taking advantage of micro-space area for reaction/detection at the tip of capillary. The chemiluminescence reaction of 1,10-phenanthroline and hydrogen peroxide was adopted and Cu(II) sample was used as a model. Three different length capillaries were inserted into the flow-type chemiluminescence detection cell made of Teflon-tube. Three samples migrated in the corresponding capillaries at the same time and mixed with CL reagent at the tip of capillary to produce chemiluminescence. The simultaneous analysis of plural samples in the present system supported the possibility that the real sample could be determined more easily, rapidly, and precisely with the calibration plots.