Magnetic resonance microimaging (MR mu I) is an outstanding technique for studying water transfers in millimetric bio-based materials in a non-destructive and non-invasive manner. However, depending on the composition of the material, monitoring and quantification of these transfers can be very complex, and hence reliable image processing and analysis tools are necessary. In this study, a combination of MR mu I and multivariate curve resolution-alternating least squares (MCR-ALS) is proposed to monitor the water ingress into a potato starch extruded blend containing 20% glycerol that was shown to have interesting properties for biomedical, textile, and food applications. In this work, the main purpose of MCR is to provide spectral signatures and distribution maps of the components involved in the water uptake process that occurs over time with various kinetics. This approach allowed the description of the system evolution at a global (image) and a local (pixel) level, hence, permitted the resolution of two waterfronts, at two different times into the blend that could not be resolved by any other mathematical processing method usually used in magnetic resonance imaging (MRI). The results were supplemented by scanning electron microscopy (SEM) observations in order to interpret these two waterfronts in a biological and physico-chemical point of view.