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基于维生素B_(12)(VB_(12))对鲁米诺-双氧水体系良好的化学发光(CL)催化活性,研究确立了一种新型毛细管电泳—化学发光(CE-CL)检测方法,用于这一重要营养物质的准确CL分析.预处理阶段,连二亚硫酸钠(Na_2S_2O_4)被确定为将VB_(12)(Co(III))转化成VB_(12)(Co(II))的适当还原剂,以使VB_(12)在luminol-H_2O_2发光体系中获得良好的催化信号.这一过程产生的CL干扰组分,则通过毛细管电泳(CE)加以分离除去.实验中,VB_(12)可被温和还原并由催化所得CL信号精确测定.采用实验室自行组建的CE-CL检测装置,该测试过程可在20 min内完成;检测下限(LOD)2×10~(-7)mol/L(S/N=3),线性范围6×10~(-7)～6×10~(-4) mol/L(r~2=0.968),相对标准偏差(RSD)2.4%(n=9).对药品中VB_(12)含量进行加标回收实验,回收率97%～106%.相较于已有关于VB_(12)的CL分析研究,本文首次考察了预还原处理中产生的干扰组分及其分离过程,以便捷操作获得更为可靠的检测数据.
Based on the good chemiluminescence (CL) catalytic activity of luminol-H 2 O 2 system with vitamin B 12 (VB 12), a new capillary electrophoresis-chemiluminescence (CE-CL) Accurate CL analysis of this important nutrient. In the pretreatment stage, sodium dithionite (Na2S2O4) was identified as a suitable reductant to convert VB 12 (Co (III)) to VB 12 (Co (II)) (12) in the luminol-H 2 O 2 luminescence system to obtain a good catalytic signal CL interference components generated in this process, then separated by capillary electrophoresis (CE) to be removed in the experiment, VB 12 can be The sample was gently reduced and accurately detected by the CL signal.Using the CE-CL detector set up by the laboratory, the test procedure can be completed within 20 min. The detection limit (LOD) is 2 × 10 -7 mol / L The linear range was from 6 × 10 -7 to 6 × 10 -4 mol / L (r = 2 = 0.968) and the relative standard deviation (RSD) was 2.4% (n = 9) The recoveries of 97% ~ 106% of VB_ (12) in pharmaceuticals were determined by the spike recovery test.Compared with the existing CL analysis of VB_ (12), we first investigated the interference groups generated in prereduction treatment Points and the separation process, to facilitate the operation to obtain Reliable detection data.