Simple and Effective HPLC Method for Elucidating Glycerol Oxidation Products.

IF 4.6 Q1 CHEMISTRY, ANALYTICAL

ACS Measurement Science Au Pub Date : 2025-05-31 eCollection Date: 2025-06-18 DOI:10.1021/acsmeasuresciau.5c00024

Eva Ng, Camilo A Mesa, Elena Mas-Marzá, Sixto Giménez

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Abstract

The glycerol electrooxidation reaction (GEOR) has been gaining increasing attention as a substitute for the oxygen evolution reaction to improve H₂ production while producing high-value-added products. During GEOR, several C₃, C₂, and C₁ species can be generated, making the detection and quantification of all these products a complex challenge that has not been fully addressed yet. Our study describes the development and optimization of a simple high-performance liquid chromatography (HPLC) method, capable not only of detecting but also simultaneously quantifying eight different GEOR products using a single diode array detector (DAD). To address possible overlapping signals, an indirect quantification approach is also proposed. The optimized method has been applied to real electrochemical GEOR systems, employing a Ni foil in alkaline media or a Pt foil in acidic media as oxidation electrocatalysts. Results show how product distributions varied significantly along with the pH, with formate being the main product in alkaline conditions (∼68% selectivity), whereas glyceraldehyde and dihydroxyacetone were the major products in acidic conditions (∼40% and ∼26%, respectively).

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简单有效的HPLC法分析甘油氧化产物。

甘油电氧化反应（GEOR）作为析氧反应的替代反应，在生产高附加值产品的同时提高H2的产率，受到越来越多的关注。在GEOR过程中，可以产生多种C3、C2和C1物质，这使得所有这些产物的检测和定量成为一项复杂的挑战，目前尚未完全解决。我们的研究描述了一种简单的高效液相色谱（HPLC）方法的开发和优化，该方法不仅可以检测而且可以使用单个二极管阵列检测器（DAD）同时定量8种不同的GEOR产品。为了解决可能的重叠信号，还提出了一种间接量化方法。该优化方法已应用于实际的电化学GEOR系统中，分别采用碱性介质中的镍箔或酸性介质中的铂箔作为氧化电催化剂。结果表明，产物分布随pH值变化显著，在碱性条件下甲酸酯是主要产物（选择性为~ 68%），而在酸性条件下甘油醛和二羟丙酮是主要产物（分别为~ 40%和~ 26%）。

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来源期刊

ACS Measurement Science Au 化学计量学-

CiteScore

5.20

自引率

0.00%

发文量

期刊介绍： ACS Measurement Science Au is an open access journal that publishes experimental computational or theoretical research in all areas of chemical measurement science. Short letters comprehensive articles reviews and perspectives are welcome on topics that report on any phase of analytical operations including sampling measurement and data analysis. This includes:Chemical Reactions and SelectivityChemometrics and Data ProcessingElectrochemistryElemental and Molecular CharacterizationImagingInstrumentationMass SpectrometryMicroscale and Nanoscale systemsOmics (Genomics Proteomics Metabonomics Metabolomics and Bioinformatics)Sensors and Sensing (Biosensors Chemical Sensors Gas Sensors Intracellular Sensors Single-Molecule Sensors Cell Chips Arrays Microfluidic Devices)SeparationsSpectroscopySurface analysisPapers dealing with established methods need to offer a significantly improved original application of the method.