Self-correcting method for the measurement of free calcium and magnesium concentrations by 1H NMR

Wallace, Matthew ORCID: https://orcid.org/0000-0002-5751-1827, Hicks, Thomas, Khimyak, Yaroslav ORCID: https://orcid.org/0000-0003-0424-4128 and Angulo, Jesus ORCID: https://orcid.org/0000-0001-7250-5639 (2019) Self-correcting method for the measurement of free calcium and magnesium concentrations by 1H NMR. Analytical Chemistry, 91 (22). pp. 14442-14450. ISSN 0003-2700

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Abstract

A method for the direct measurement of free Ca2+ and Mg2+ concentrations in the range of 1–100 mM by NMR spectroscopy is demonstrated. The method automatically corrects for the effect of ionic strength on the activity of the species in solution and works satisfactorily even when significant concentrations of competitive ions are present. The method requires only the measurement of the 1H chemical shifts of our reporter ligands, glycolate and sulfoacetate, and is easily implemented using NMR imaging techniques. As a proof of concept, we extract the thermodynamic binding constants and conformer distributions of analyte ligands using an in situ ion gradient. Existing approaches for the measurement of free Ca2+ or Mg2+ concentrations by NMR operate only at very low ion concentrations or else require careful recalibration for different sample conditions. By providing the free Ca2+ or Mg2+ concentrations, the proposed methodology significantly enhances the information obtainable via NMR investigations of ion-responsive systems.

Item Type:	Article
Faculty \ School:	Faculty of Science > School of Pharmacy (former - to 2024)
UEA Research Groups:	Faculty of Science > Research Groups > Pharmaceutical Materials and Soft Matter
Depositing User:	LivePure Connector
Date Deposited:	04 Nov 2019 12:30
Last Modified:	16 Dec 2024 01:30
URI:	https://ueaeprints.uea.ac.uk/id/eprint/72862
DOI:	10.1021/acs.analchem.9b03008

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