Debranched cassava starch crystallinity determination by Raman spectroscopy: Correlation of features in Raman spectra with X-ray diffraction and 13C CP/MAS NMR spectroscopy

► Analyzed starches of different crystallinities using X-ray diffraction and 13C CP/MAS NMR spectroscopy. ► Correlated calculated crystallinities with FT-Raman spectra. ► Strong linear correlation exists between crystallinity and integrated areas of Raman bands. ► FT-Raman spectroscopy is a promising tool for rapid determination of starch crystallinity. Because starch crystallinity influences the physical, mechanical, and technological aspects of numerous starch-based products during production and storage, rapid techniques for its assessment are vital. Samples of different levels of crystallinity were obtained by debranching gelatinized cassava starch, followed by subjection to various hydrothermal treatments. The recrystallized products were further subjected to partial hydrolysis with a mixture of α-amylase and glucoamylase prior to freeze–drying. Crystallinities were determined using X-ray diffraction (XRD) and 13C CP/MAS NMR spectroscopy, and correlated with FT-Raman spectra features. XRD crystallinities ranged between 0 and 58%, and agreed with crystalline-phase fractions (R2=0.99) derived from the respective 13C CP/MAS NMR spectra. A strong linear correlation was found between crystallinities and integrated areas of the skeletal mode Raman band at 480cm−1 (R2=0.99). With appropriate calibration, FT-Raman spectroscopy is a promising tool for rapid determination of starch crystallinity.