Structural characterization of tin in toothpaste by dynamic nuclear polarization enhanced 119Sn solid-state NMR spectroscopy
Rick W. Dorn,
Scott L. Carnahan,
Chi-yuan Cheng,
Long Pan,
Zhigang Hao () and
Aaron J. Rossini ()
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Rick W. Dorn: US Department of Energy Ames National Laboratory
Scott L. Carnahan: US Department of Energy Ames National Laboratory
Chi-yuan Cheng: Colgate-Palmolive Company
Long Pan: Colgate-Palmolive Company
Zhigang Hao: Colgate-Palmolive Company
Aaron J. Rossini: US Department of Energy Ames National Laboratory
Nature Communications, 2023, vol. 14, issue 1, 1-11
Abstract:
Abstract Stannous fluoride (SnF2) is an effective fluoride source and antimicrobial agent that is widely used in commercial toothpaste formulations. The antimicrobial activity of SnF2 is partly attributed to the presence of Sn(II) ions. However, it is challenging to directly determine the Sn speciation and oxidation state within commercially available toothpaste products due to the low weight loading of SnF2 (0.454 wt% SnF2, 0.34 wt% Sn) and the amorphous, semi-solid nature of the toothpaste. Here, we show that dynamic nuclear polarization (DNP) enables 119Sn solid-state NMR experiments that can probe the Sn speciation within commercially available toothpaste. Solid-state NMR experiments on SnF2 and SnF4 show that 19F isotropic chemical shift and 119Sn chemical shift anisotropy (CSA) are highly sensitive to the Sn oxidation state. DNP-enhanced 119Sn magic-angle turning (MAT) 2D NMR spectra of toothpastes resolve Sn(II) and Sn(IV) by their 119Sn chemical shift tensor parameters. Fits of DNP-enhanced 1D 1H → 119Sn solid-state NMR spectra allow the populations of Sn(II) and Sn(IV) within the toothpastes to be estimated. This analysis reveals that three of the four commercially available toothpastes contained at least 80% Sn(II), whereas one of the toothpaste contained a significantly higher amount of Sn(IV).
Date: 2023
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DOI: 10.1038/s41467-023-42816-z
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