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Unraveling the Cyclization of l-Argininosuccinic Acid in Biological Samples: A Study via Mass Spectrometry and NMR Spectroscopy.
Analytical Chemistry ( IF 6.7 ) Pub Date : 2020-08-21 , DOI: 10.1021/acs.analchem.0c01420 Maricruz Mamani-Huanca 1 , Ana Gradillas 1 , Ángeles López-Gonzálvez 1 , Coral Barbas 1
Analytical Chemistry ( IF 6.7 ) Pub Date : 2020-08-21 , DOI: 10.1021/acs.analchem.0c01420 Maricruz Mamani-Huanca 1 , Ana Gradillas 1 , Ángeles López-Gonzálvez 1 , Coral Barbas 1
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Since l-argininosuccinic acid (ASA) is the characteristic biomarker for the diagnosis of certain diseases, its reliable detection in complex biological samples is necessary to obtain a complete evaluation with greater specificity and accuracy. ASA can undergo intramolecular cyclization, yielding an equilibrium with the resulting cyclic forms, which can predominate under different analytical conditions. In this work, the appearance and transformation of the different forms of ASA have been studied and a strategy for targeted screening analysis of ASA and its cyclic forms using capillary electrophoresis-electrospray ionization-time-of-flight mass spectrometry (CE-ESI-TOF-MS) has been developed. The data and spectra obtained allowed us to gain further insight into accurate identification, concluding that there is a dynamic equilibrium depending on the pH. Moreover, one- and two-dimensional NMR spectroscopy experiments have allowed us to determine the predominant tautomeric structure for the major cyclic ASA derivative, confirming the importance of intramolecular hydrogen bonds.
中文翻译：
揭开生物样品中l-精氨酸琥珀酸的环化：通过质谱和NMR光谱的研究。
由于升-精氨酸琥珀酸（ASA）是诊断某些疾病的特征性生物标志物，在复杂的生物样品中进行可靠的检测对于获得具有更高特异性和准确性的完整评估是必不可少的。ASA可以进行分子内环化，从而与所形成的环状形式保持平衡，在不同的分析条件下，环状形式可能占主导。在这项工作中，研究了不同形式的ASA的出现和转化，并提出了使用毛细管电泳-电喷雾电离飞行时间质谱（CE-ESI-TOF）对ASA及其环状形式进行靶向筛选分析的策略-MS）已开发。所获得的数据和光谱使我们能够进一步深入了解准确的鉴定，并得出结论，取决于pH值存在动态平衡。
更新日期：2020-10-06
中文翻译：
揭开生物样品中l-精氨酸琥珀酸的环化：通过质谱和NMR光谱的研究。
由于升-精氨酸琥珀酸（ASA）是诊断某些疾病的特征性生物标志物，在复杂的生物样品中进行可靠的检测对于获得具有更高特异性和准确性的完整评估是必不可少的。ASA可以进行分子内环化，从而与所形成的环状形式保持平衡，在不同的分析条件下，环状形式可能占主导。在这项工作中，研究了不同形式的ASA的出现和转化，并提出了使用毛细管电泳-电喷雾电离飞行时间质谱（CE-ESI-TOF）对ASA及其环状形式进行靶向筛选分析的策略-MS）已开发。所获得的数据和光谱使我们能够进一步深入了解准确的鉴定，并得出结论，取决于pH值存在动态平衡。
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