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首次报道毛细管离子分析的新型研究技术─—自行组装的毛细管电泳化学发光检测器,将内径为50μm的电泳毛细管经刻蚀插入内径为530μm的反应管,内径为120μm的试剂管通过聚四氟乙烯三通将试剂引入反应管中,反应管上的检测窗定位于光电倍增管前,使光信号尽可能多地被接收。金属离子催化鲁米诺-过氧化氢发光是较灵敏的化学发光研究体系,但干扰严重。高效液相色谱分离对象有限,分离效率不十分理想。本系统成功地基线分离了Co ̄(2+)、Cu ̄(2+)、Ni ̄(2+)、Fe ̄(3+)、Mn ̄(2+)五种金属离子,分离迅速(8分钟内),峰形非常尖锐,理论塔板数达10 ̄5数量级,对Co ̄(2+)的检测限达5×10 ̄(-13)mol/L(20zmol),显著低于目前报道的最灵敏结果(10 ̄(-11)mol/L),对Cu ̄(2+)、Ni ̄(2+)、Fe ̄(3+)、Mn ̄(2+)的检测限分别为2amol、80amol、740amol、100fmol,灵敏度明显优于毛细管离子分析中常用的光度检测法。该研究的新颖之处在于将发光试剂鲁米诺作为分离电解质溶液的组分,利用金属离子的快速催化动力学机理,使离子与发光试剂在检测窗口相遇迅速产生光信号,这?
First report of capillary ion analysis of a new type of research ─ ─ self-assembly capillary electrophoresis chemiluminescence detector, the diameter of 50μm electrophoresis capillary was inserted into the inner diameter of 530μm reaction tube, the inner diameter of the reagent tube 120μm by polytetrafluoroethylene The tee introduces the reagent into the reaction tube, and the detection window on the reaction tube is positioned in front of the photomultiplier tube so that the optical signal is received as much as possible. Metal ion-catalyzed luminol-H2O2 luminescence is a more sensitive chemiluminescence research system, but the interference is serious. High performance liquid chromatography separation of the object is limited, the separation efficiency is not very good. The system successfully separated five metal ions Co ~ (2 +), Cu ~ (2+), Ni ~ (2+), Fe ~ (3 +) and Mn ~ (2+) The results show that the detection limit of Co ~ (2+) is 5 × 10 ~ (-13) mol / L (20zmol), which is significantly lower than the most sensitive results reported so far The sensitivity of Cu 2+, Ni 2+, Fe 3+ and Mn 2+ was 2 amol, 80 amol, 740 amol and 100 fmol, respectively Commonly used photometric detection in capillary ion analysis. The novelty of this study lies in that luminol, a luminescent reagent, is used as a component of separating the electrolyte solution and utilizes the rapid catalytic kinetic mechanism of metal ions to rapidly generate optical signals when the ions and luminescent reagents meet in the detection window.