This study presents the first liquid chromatography method for the quantitative and qualitative analysis of highly reactive oxoammonium cations based on a simple derivatization reaction. Rapid 1,2-electrophilic addition reactions with olefins were used to transform these reactive species into analyzable derivates. Three model substances were chosen to represent each of the main application fields of oxoammonium cations and to demonstrate the versatility of the method. The measuring protocol was validated according to the ICH and USP guidelines. The method revealed an excellent linearity (R² = 0.9980–0.9990) with a low limit of detection (0.16–0.14 mmol L⁻¹) and a low limit of quantification (0.55–0.43 mmol L⁻¹). The protocol was finally used to determine the oxoammonium cations in the presence of their corresponding radical, showing a robustness against impurity concentration of up to approx. 30%.

本研究提出了第一种基于简单衍生反应对高活性氧代铵阳离子进行定量和定性分析的液相色谱方法。使用与烯烃的快速 1,2-亲电加成反应将这些活性物质转化为可分析的衍生物。选择了三种模型物质来代表氧铵阳离子的每个主要应用领域并证明该方法的多功能性。测量方案根据 ICH 和 USP 指南进行了验证。该方法显示出极好的线性 ( R ²  = 0.9980–0.9990)，检测下限 (0.16–0.14 mmol L ^-1 ) 和定量下限 (0.55–0.43 mmol L ^-1）。该方案最终用于在存在相应自由基的情况下确定氧代铵阳离子，显示出对高达约 30%。