Physico-chemical properties study of solid state inulin

The aim of this research is to understand the solid state physical properties of inulin in regards to the spray-drying treatments. In this context, inulin powders were produced by pilot spray-drying a commercial inulin dispersion under various feed (Tfeed) and inlet air (Tin) temperatures. More particularly, the amorphous and crystalline properties of the powders were studied by developing different fine characterization tools, such as modulated differential scanning calorimetry or powder X-ray diffraction. When the temperature of the inulin – water systems increased, the crystallinity of the powder decreased. To a smaller extent, this tendency is also observed with the increase of the inlet air temperature of the spray drier. For example, an amorphous powder is obtained with a Tfeed of 90°C whatever the Tin (comprised between 120 and 230°C); whereas for a Tfeed of 80°C, a Tin of 230°C is necessary to obtain the same result. Adsorption isotherms were established on four powders covering a large range of crystallinity (crystallinity index from 0 to 92). The Guggenheim – Anderson – de Boer model was fitted to the experimental data. As the water content of the powders increased, the glass transition of inulin decreased. When the Tg droped below the storage temperature (20°C for example), the powders crystallized and underwent clumping phenomenon. Under these conditions, a continuous hard mass was observed for the amorphous powders; while their semi-crystalline counterparts were agglomerated but friable. To understand these changes, a kinetic study of the physical properties evolution and stability of an amorphous powder as a function of its water content was realized. These results allowed to correlate the Tg – water content relationship to the evolution of the powder’s behaviour, such as stickiness or hardening during storage

Impact of the crystallisation pathway of inulin on its mono-hydrate to hemi-hydrate thermal transition

In this paper, we present the thermal properties of two inulins obtained from different crystallisation pathways. One was obtained by fractional precipitation of a saturated inulin solution and the second was from the crystallisation of a solid amorphous mulin. The thermal analyses were conducted by temperature resolved wide angle X-ray scattering (TRWAXS), differential scanning calorimetry (DSC) and thermogravimetry (TG). Although at room temperature both inulins presented similar X-ray diffractogram patterns characteristic of the mono-hydrate polymorph, they differed considerably by their thermal properties. During heating, a difference in the mono-hydrate to the hemi-hydrate polymorph transition occurred. Thermogravimetric analysis suggested a difference in the water mobility inside the material which had an impact on the thermal properties and hydrate transition of the crystalline inulin. (C) 2009 Elsevier Ltd. All rights reserved

Isolation and identification of inulooligosaccharides resulting from inulin hydrolysis

In this study, inulooligosaccharides (F-n-type inulin) resulting from the endo-inulinase hydrolysis of globe artichoke inulin were purified and characterized. The aim was to produce F-n oligomer standards with the intention of identifying them in the complex inulin chromatogram. Inulin was extracted from globe artichoke and presented a high average degree of polymerization (DP) of about 80 as determined by high-performance anion exchange chromatography coupled with pulsed amperometric detection (HPAEC-PAD). This inulin was hydrolyzed by a commercial endo-inulinase yielding a product with a very high F-n/GF(n), molecule ratio, thus limiting the interference of GF(n) during the purification process. High performance size exclusion chromatography was used to individually isolate and collect each retention peak corresponding to a specific oligomer. The purity of these fractions was checked by HPAEC-PAD and showed that relatively pure molecules were produced. Electrospray ionization mass spectrometry allowed the molecular weight determination of these purified oligomers and ascertained their DP as F-2, F-3 and F-4. These F2-4 standards were used with glucose, fructose, sucrose and GF(2-4) (commercially available) to spike commercial oligofructose products in order to determine the elution profile in the HPAEC-PAD chromatogram