NDA柱前衍生毛细管电泳高灵敏安培检测组胺

Determination of Histamine by Capillary Electrophoresis with Pre-column NDA Derivatization and Amperometric Detection

本文提出了毛细管电泳 2,3 萘二甲醛(NDA)柱前衍生高灵敏安培检测组胺的新方法,对衍生反应条件和电泳分析条件,包括衍生试剂浓度、衍生溶液的pH值、衍生反应时间、分离介质的pH值、进样时间和分离电压进行了优化,确定衍生溶液pH值为9.0,NDA浓度为5.0×10-4mol/L,CN-浓度为2.5×10-3mol/L时的衍生效果最佳;10mmol/LTris H3PO4(pH5.0)为最佳电泳缓冲液,检测电位为0.7V(vs.SCE)时,组胺检出限达6.8×10-8mol/L(S/N=3),较不衍生测定法灵敏度提高6倍,为测定痕量组胺提供了一个新方法。

A method using capillary zone electrophoresis by pre-column derivatization with Naphthalene-2,3-dicarboxaldehyde (NDA)/CN^(-) and amperometric detection at a carbon fiber electrode was developed for the determination of histamine. The derivatization reaction conditions, including the concentration of NDA and cyanide, pH value of derivatization buffer and reaction time and separation conditions were investigated. The optimum derivatization conditions were 5.0×10^(-4) mol/L and 2.5×10^(-3) mol/L for the concentration of NDA and cyanide respectively and 9.0 for the pH value of derivatization buffer. The optimum separation conditions were 10 mmol/L Tris-H_(3)PO_(4) (pH 5.0) for the running buffer and 15 kV for the separation voltage. The detection limit was 6.8×10^(-8) mol/L (S/N=3) with the detection potential of 0.7 V vs. SCE.