Probing structural features in potato starch granules at moderate hydration through the modelling of ¹H->¹³C...

The structural arrangement of starch polymers in presence of water is known to impact the functional properties of starchy products. In this study, the hydration of potato starch granules was investigated at the molecular level through various ¹H->¹³C polarization transfer solid-state Nuclear Magnetic Resonance (ss-NMR) experiments. The impact of increasing the water content from 12.3 % to 45.9 % was assessed using ¹³C Cross Polarization Magic Angle Spinning (CPMAS), Variable Contact Time (VCT-CPMAS), Variable Spin Lock (VSL-CPMAS), and T One Rho QUEnching (TORQUE) NMR sequences. Of these, VCT-CPMAS proved to be the most promising. When applied with an optimal number of contact times, it enabled the application of several mathematical models that provided detailed insights into the structuring of protons in the hydrated potato starch granules. At low hydration (12.3 %), the models enabled various structural domains to be distinguished, which we suggest are associated with helical and amorphous structures. At moderate hydration (45.9 %), we tested two fitting models. Two pools of protons were revealed, corresponding to loosely ordered structures on the scale of tens of nanometers. These findings suggest varying water distribution during starch hydration and are likely to indicate variable hydration levels in the multilamellar amorphous structures of starch granules.