Self-Correcting Method for the Measurement of Free Calcium and Magnesium Concentrations by 1H NMR

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 concentr...

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Veröffentlicht in:	Analytical chemistry (Washington) 2019-11, Vol.91 (22), p.14442-14450
Hauptverfasser:	Wallace, Matthew, Hicks, Thomas, Khimyak, Yaroslav Z, Angulo, Jesús
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Sprache:	eng
Schlagworte:	Analytical chemistry Calcium Calcium ions Chemistry Imaging techniques Ionic strength Ligands Magnesium Magnetic resonance spectroscopy NMR NMR spectroscopy Nuclear magnetic resonance Organic chemistry
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creator	Wallace, Matthew Hicks, Thomas Khimyak, Yaroslav Z Angulo, Jesús
description	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.
doi_str_mv	10.1021/acs.analchem.9b03008
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Chem</addtitle><date>2019-11-19</date><risdate>2019</risdate><volume>91</volume><issue>22</issue><spage>14442</spage><epage>14450</epage><pages>14442-14450</pages><issn>0003-2700</issn><eissn>1520-6882</eissn><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. 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subjects	Analytical chemistry Calcium Calcium ions Chemistry Imaging techniques Ionic strength Ligands Magnesium Magnetic resonance spectroscopy NMR NMR spectroscopy Nuclear magnetic resonance Organic chemistry
title	Self-Correcting Method for the Measurement of Free Calcium and Magnesium Concentrations by 1H NMR
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