*3.6. Low Field Nuclear Magnetic Resonance Spectroscopy Measurements*

To identify possible differences in the water distribution (or rather proton populations) in the bread supplemented with different concentrations and types of CDs, bread samples from day 1,4,7,10,14, and 17 were analyzed by <sup>1</sup>H low field nuclear magnetic resonance (LF-NMR) spectroscopy (MQR Spectro-P spectrometer, Oxford Instruments, Oxfordshire, UK, operating at 20 MHz). Approximately 1.5 g of bread crumb was sampled from a slice of bread using a cork borer and placed into a glass tube for NMR measurements. Data were collected using a Carr–Purcell–Meiboon–Gill (CPMG) sequence at 25 ◦C with the parameters: Recycle delay of 5 s, τ-delay of 100 µs, and 16 scans averaged. Data from 6000 echoes were acquired with a receiver gain of 5.0. All measurements were prepared in triplicates on distinct samples. Transverse relaxation times (T2n) of different relaxation components were obtained using an in-house MATLAB (version R2019a, The Math-Works) script designed for fitting the relaxation curves to a series of exponential decays according to Equation (1).

$$I(t) = \sum\_{n=1}^{N} M\_n \cdot e^{-t/T\_{2u}} \tag{1}$$

In which *I*(*t*) is the echo intensity as a function of relaxation time, *N* is the number of relaxation components, the transverse relaxation time for site *n* is *T2n*, and the corresponding abundance is *Mn. N* is determined by visual inspection of the residuals after model fitting. Each LF-NMR recording was fitted individually. All *Mn*-values were presented as percentage of total intensity to eliminate sample size differences.
