Xu Lihua, Huang Biling, Hou Zhiying, Huang Shaohua, Zhao Yufen
Institute of Drug Discovery Technology, Ningbo University, Ningbo, 315211, P.R. China.
Qian Xuesen Collaborative Research Center of Astrochemistry and Space Life Sciences, Ningbo University, Ningbo, 315211, P.R. China.
Anal Chem. 2023 Feb 7;95(5):3012-3018. doi: 10.1021/acs.analchem.2c04949. Epub 2023 Jan 27.
F NMR has been extensively used in simultaneous analysis of multicomponent due to its 100% natural isotope abundance, high NMR-sensitivity, and wide-range chemical shifts. The solvent effects are usually observed in NMR spectroscopy and cause large changes in F chemical shifts. Herein, we propose that the simultaneous analysis of a complex mixture can be achieved using solvent effects F NMR spectroscopy, such as a mixture solution of amino acids (AAs). AAs are not only cell-signaling molecules, but are also considered as biomarkers of some diseases. Hence, the analysis of AAs is important for human health and the diagnosis of diseases. In this work, the key to the success of sensing 19 biogenic AAs is the use of 2-fluorobenzaldehyde (2FBA) as a highly sensitive derivatizing agent and solvent effects to produce distinguishable F NMR signals. As a result, the resolution of F NMR spectroscopy of multiple 2FBA-labeled AAs is obviously higher than other methods based on F NMR. Moreover, 14 and 18 AAs can be satisfactorily differentiated and unambiguously identified in different complicated media supporting the growth of mammalian cells. Furthermore, quantification of the concentration of AAs can be made, and the limit of detection reaches 10 μM. Our work provides new insights into the simultaneous analysis of a multicomponent mixture based on solvent effects by F NMR spectroscopy.
氟核磁共振(F NMR)因其100%的天然同位素丰度、高核磁共振灵敏度和宽范围的化学位移,已被广泛用于多组分的同时分析。在核磁共振光谱中通常会观察到溶剂效应,并且会导致氟化学位移发生很大变化。在此,我们提出可以使用溶剂效应氟核磁共振光谱来实现对复杂混合物的同时分析,例如氨基酸(AAs)的混合溶液。氨基酸不仅是细胞信号分子,还被视为某些疾病的生物标志物。因此,氨基酸的分析对人类健康和疾病诊断很重要。在这项工作中,成功检测19种生物源性氨基酸的关键在于使用2-氟苯甲醛(2FBA)作为高灵敏度衍生剂以及利用溶剂效应来产生可区分的氟核磁共振信号。结果,多种2FBA标记氨基酸的氟核磁共振光谱分辨率明显高于其他基于氟核磁共振的方法。此外,在支持哺乳动物细胞生长的不同复杂介质中,可以令人满意地区分并明确鉴定出14种和18种氨基酸。此外,还可以对氨基酸浓度进行定量,检测限达到10 μM。我们的工作为基于溶剂效应通过氟核磁共振光谱对多组分混合物进行同时分析提供了新的见解。