Laboratory of Analytical Chemistry, Faculty of Pharmaceutical Sciences, Sojo University, Nishi-ku, Kumamoto, Japan.
Anal Chem. 2013 Jul 16;85(14):6833-9. doi: 10.1021/ac401002v. Epub 2013 Jun 27.
Measuring the superoxide anion radical (superoxide) with high sensitivity is necessary to clarify the mechanisms of diseases for the development of methods for their prophylaxes, diagnoses, and therapies. The chemiluminescence technique using Cypridina luciferin analogues such as MCLA and CLA is currently the most sensitive method available. Using large concentrations of these reagents, however, leads to increases in background levels due to spontaneous luminescence of the reagent, which is a limitation of this method. This study demonstrated that the superoxide-induced chemiluminescence of MCLA or CLA was markedly enhanced by adding a cyclic nitroxyl radical to the reaction medium. When MCLA was measured spectrophotometrically, the nitroxyl radical was shown to increase the reaction rate of superoxide and MCLA without altering their stoichiometry, whereas consumption of the nitroxyl radical was negligible, as determined by electron paramagnetic resonance (EPR) spectroscopy. These observations indicate that the nitroxyl radical catalytically enhanced the reaction between superoxide and MCLA, resulting in an enhancement in superoxide-dependent MCLA chemiluminescence. This method is applicable to biological systems such as superoxide-generation by neutrophils. The inclusion of the cyclic nitroxyl radical in a sample solution contributed to reductions in the concentration of the chemiluminescence reagent, thereby decreasing background levels. The catalytic mechanism was also discussed.
测定超氧阴离子自由基(超氧)的高灵敏度对于阐明疾病机制、开发预防、诊断和治疗方法是必要的。目前,使用海肾荧光素类似物(如 MCLA 和 CLA)的化学发光技术是最敏感的方法。然而,使用这些试剂的大浓度会由于试剂的自发发光而导致背景水平升高,这是该方法的一个限制。本研究表明,向反应介质中添加环状氮氧自由基可显著增强 MCLA 或 CLA 的超氧诱导化学发光。当通过分光光度法测量 MCLA 时,氮氧自由基被证明可以增加超氧和 MCLA 的反应速率,而不改变它们的化学计量,而电子顺磁共振(EPR)光谱表明氮氧自由基的消耗可以忽略不计。这些观察结果表明,氮氧自由基催化增强了超氧和 MCLA 之间的反应,导致超氧依赖的 MCLA 化学发光增强。该方法适用于生物系统,例如中性粒细胞产生的超氧。环状氮氧自由基包含在样品溶液中有助于降低化学发光试剂的浓度,从而降低背景水平。还讨论了催化机制。