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

采用毛细管电泳法和化学发光检测器对酚类化合物进行了分析。过氧草酸化学发光剂与丹磺酰氯联用作为标记剂。考察了试剂浓度、标记方法和化学发光检测池的性能，以实现对酚类化合物的灵敏检测。6种酚类化合物(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)的测定范围为3个数量级，检出限为10-7M量级，检出限约为普通荧光检测器的10倍。用含有十二烷基硫酸钠和乙腈的流动缓冲溶液对15种酚类化合物进行了分离，结果令人满意。毛细管电泳法、电泳法与化学发光法、柱浓缩法的结合，为本系统应用于地表水、回用水等实际样品提供了可能；同时，利用毛细管末端的微空间区域进行反应/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，以铜(II)样品为模型。将三根不同长度的毛细管插入到由特氟龙管制成的流动化学发光检测池中。三个样品同时在相应的毛细管中迁移，并与毛细管顶端的CL试剂混合产生化学发光。在本系统中对多个样品的同时分析支持了使用校准图更容易、更快速、更准确地测定真实样品的可能性。

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.