Reliable and Accessible Methods for Urea Quantification in Co-Reduction of Carbon-Dioxide- and Nitrogen-Containing Species

Yan Zhang, Gefei Huang, Haichuan Zhang, Xiaoyi Qiu, Guimei Liu, Yinuo Wang,Juhee Jang, Yian Wang,Zidong Wei,Zongwei Cai,Minhua Shao

Chem Catalysis（2025）

School of Chemistry and Chemical Engineering

Cited 0|Views4

Abstract

Electrocatalytic urea synthesis by the co-reduction of CO2 and nitrogen sources under mild conditions offers an attractive alternative to the conventional protocol. However, the quantification of urea poses significant challenges because of low yields and diverse byproducts, thereby raising concerns regarding the reliability of catalyst performance. This study systematically assesses the commonly used methods (urease, diacetyl monoxime, and 1H-NMR) in real electrochemical systems and identifies their potential limitations. We then propose an advanced analytical platform that uses ultra-high-performance liquid chromatography coupled with high-resolution mass spectrometry (UHPLC-HRMS) to quantify urea in electrolytes. This method exhibits high sensitivity, even at ultralow urea concentrations of 0.01 μg mL−1, without compromising accuracy in the presence of byproducts. Its reliability is validated through a series of experimental cases, eliminating the occurrence of false positives. These findings contribute to establishing a benchmark for quantifying urea in electrosynthesis, facilitating the development of efficient electrocatalysts.

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Key words

electrocatalytic synthesis,urea quantification,ultra-high-performance liquid chromatography,CO2 reduction,nitrogen sources,C–N coupling,nitrate reduction

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【要点】：该论文提出了一种可靠且易于使用的高效尿素量化方法，用于二氧化碳和含氮物种共还原过程中的电催化尿素合成，提高了催化剂性能评估的准确性。

【方法】：作者采用了一种结合超高效液相色谱与高分辨率质谱（UHPLC-HRMS）的先进分析平台，对尿素在电解质中的含量进行量化。

【实验】：通过在真实电化学系统中对常用量化方法（脲酶、二乙酰一肟和1H-NMR）进行评估，并使用UHPLC-HRMS方法进行实验验证，证明了该方法在痕量尿素浓度下的高灵敏度和准确性，实验数据集名称未在文中提及。