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Tempol radical

Manufactured by Merck Group

TEMPOL is a stable nitroxide radical compound. It is a powerful antioxidant and spin-label used in various research applications, including electron paramagnetic resonance (EPR) spectroscopy and as a model compound for studying radical reactions.

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3 protocols using tempol radical

1

Dynamic Nuclear Polarization of 13C-Lactate

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HP [1-13C] lactate was prepared as previously described34 . Briefly, frozen beads containing sodium [1-13C] L-lactate solution (45–55% (w/w) in H2O, Sigma Aldrich) and d8-glycerol (Sigma Aldrich) were mixed 1:1 (w/w). The sample was dynamically polarised using TEMPOL radical (58 mM, Sigma Aldrich) as polarising agent on a custom-designed 7 T DNP polariser operating at 197 GHz/1.00 ± 0.05 K38 (link) for 2 h, then rapidly dissolved in 5 mL of superheated D2O and transferred within 2 s into the separator/infusion pump39 (link), which was positioned inside the magnet bore. The [1-13C] lactate polarisation measured at the separator was 15.6 ± 2.0% (n = 5). A bolus of the solution was automatically infused over 3 s through the catheterised mouse femoral vein as previously described40 (link).
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2

Hyperpolarized Proton NMR Spectroscopy

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A solution of 3 M [2- 13 C]sodium acetate in the glass-forming mixture
H 2 O/D 2 O/glycerol- d8 (1/3/6 v/v/v ) was doped with 50 mM TEMPOL radical (all compounds purchased from Sigma-Aldrich) and sonicated for  10 min. Paramagnetic TEMPOL radicals were chosen to polarize 1 H spins
most efficiently under our d DNP conditions.
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3

Glassy H2O/DMSO-d6 Radical Sample

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A liquid glass-forming mixture of H2O/DMSO-d6 (1/5 v/v) was doped with 50 mM TEMPOL radical (all compounds purchased from Sigma-Aldrich) and sonicated for ~2 minutes. This sample is referred to as I from here onwards. The concentration of water protons was ~9.25 M. DMSO-d6 was chosen over glycerol-d8 due to the wider availability of ~100% deuterated DMSO-d6 products. The deuteration level of DMSO-d6 used in experiments was 99.96%, which indicates a residual DMSO-d6 proton concentration of ~44 mM. Consequently, only ~0.5% of 1 H spins belong to the glassing agent and as such the 1 H NMR signal observed largely originates from that of water. Lower ratios of H2O/DMSO-d6 did not result in a glassy sample upon freezing [30] (see the Electronic Supporting Information (ESI) for more details).
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