邻苯二甲酰化学发光法测定羟自由基的产生：在自然系统中的修改和改进,Analytical Chemistry

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邻苯二甲酰化学发光法测定羟自由基的产生：在自然系统中的修改和改进
Analytical Chemistry ( IF 6.7 ) Pub Date : 2010-12-10 00:00:00 , DOI: 10.1021/ac1022748
Christopher J. Miller ₁ , Andrew L. Rose ₁ , T. David Waite ₁

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羟基自由基是通过与天然和人为系统有关的各种过程形成的。在这里，我们报告了一种基于酞酰肼羟基化成5-羟基-2,3-二氢-1,4-酞嗪二酮的简单而灵敏的触发化学发光方法的进展，该方法在碱性条件下被氧化时会发出化学发光。Cu（III）被用作氧化剂，并且显示出对可能遇到的一系列干扰相对不敏感。该方法已通过使用水的γ辐射作为羟基自由基的主要来源进行了标准化，并开发了使用Fenton化学方法的便捷的二次校准程序。检测限从7.4 nM（在pH 3时）和6.2 nM（在pH 8时）变化。1）由于邻苯二甲酰肼探针和溴化物之间存在羟基竞争，因此在简单的10 mM NaCl基质中在人工海水介质中累积的羟基自由基产生量约为30 nM。该方法已用于表征用于校准的Fenton系统的动力学，并且在数小时的时间范围内显示与该过程的已发布模型一致。还介绍了该方法在一系列基质中的应用以及用于光化学研究的方法。

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Phthalhydrazide Chemiluminescence Method for Determination of Hydroxyl Radical Production: Modifications and Adaptations for Use in Natural Systems

The hydroxyl radical is formed through a variety of processes pertinent to natural and anthropogenic systems. Here we report development of a simple and sensitive trap-and-trigger chemiluminescence method based upon the hydroxylation of phthalhydrazide to 5-hydroxy-2,3-dihydro-1,4-phthalazinedione, which emits chemiluminescence when oxidized under alkaline conditions. Cu(III) is employed as an oxidant and is shown to be relatively insensitive to a range of interferences likely to be encountered. The method has been standardized by use of γ-radiolysis of water as a primary source of hydroxyl radical, with a convenient secondary calibration procedure developed that uses Fenton chemistry. Detection limits varied from 7.4 nM (at pH 3) and 6.2 nM (at pH 8.1) of accumulated hydroxyl radical production in a simple 10 mM NaCl matrix to around 30 nM in an artificial seawater medium, due to competition for hydroxyl between the phthalhydrazide probe and bromide. The method has been used to characterize the kinetics of the Fenton system employed for calibration and is shown to be consistent with published models of this process over time scales of several hours. The application of this method to a range of matrices and for photochemical studies is also described.

更新日期：2010-12-10

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