Related Experiment Video
Updated: Sep 6, 2025

A Package of Established Analytical Tools to Investigate the Solid-State Alteration of Lipid-Based Excipients
Published on: August 9, 2022
Effect of stabilization and fatty acids chain length on the crystallization behavior of interesterified blends during
Mayanny Gomes da Silva1, Kamila Ramponi Rodrigues de Godoi1, Lisandro Pavie Cardoso2
1Department of Food Engineering and Technology, School of Food Engineering, University of Campinas, 80 Monteiro Lobato St, Campinas, SP 13083-862, Brazil.
Abstract:
In this work, we studied the influence of fatty acid chain length and crystallization temperature on the crystallization behavior during the storage of binary blends modified by chemical interesterification. The blends were produced with soybean oil and fully hydrogenated oils from palm kernel, palm, soybean, microalgae, and crambe, evaluated separately, at a ratio of 50:50 (% w/w). The blends were crystallized by two crystalline stabilization methods. In method I, the samples were maintained at 25 °C for 24 h before the analyses. In method II, the samples were maintained at 5 °C for 24 h, followed by crystalline stabilization at 25 °C for 24 h before the analyses. The interesterification reaction caused considerable changes in the TAGs profile with increasing asymmetric TAGs. These TAGs changes promoted an increase in the crystallization induction time, a decrease in the maximum solids content, and changes in crystals morphology. The increase in the FAs chain length promoted the increased nucleation rate that influenced morphology crystals. Method II promoted a reduction in the medium diameter of crystals and the appearance of the β phase with storage time. For crystallization carried out at higher temperatures (method I), we observed that β' was favored. Unusual polymorphic transitions were observed with storage time in samples with higher tristearin content. We identified clear correlations between the predominance of β' phase in the interesterified blends and TAGs of S2U and SU2-type. In addition, the blends with a more diverse range of fatty acids concerning chain size also showed the β' polymorph. β polymorph, on the other hand, was associated with symmetric TAGs, S3 and U3, and CN-54 type TAG. In this study, we used the Rietveld method to quantify the polymorphs and amorphous content in the blends before and after the randomization reaction. This approach allowed a deeper understanding of the crystalline behavior in the blends, which would be difficult to achieve by performing only a visual analysis of the X-ray diffractograms.
Related Concept Videos
Carboxylic Acids to Esters: Acid-Catalyzed (Fischer) Esterification Overview
Carboxylic Acids to Esters: Acid-Catalyzed (Fischer) Esterification Mechanism
Recrystallization: Solid–Solution Equilibria
Physical Properties of Carboxylic Acid Derivatives
Among the carboxylic acid derivatives, the boiling points of acid chlorides and esters are very similar and are the lowest in the series. Acid anhydrides have slightly higher boiling...
Polymer Classification: Stereospecificity
Polymer Classification: Crystallinity
Crystalline domains are the regions where polymer chains are aligned in an orderly manner and held together in proximity by intermolecular forces. For example, chains in the crystalline domains of polyethylene and nylon are bound together by van der Waals...

