Crystallization and polymorphic behavior of shea stearin and the effect of removal of polar components

Authors


Correspondence: Dr. Andrew G. F. Stapley, Department of Chemical Engineering, Loughborough University, Leicestershire, LE11 3TU, UK

E-mail: a.g.f.stapley@lboro.ac.uk

Fax: +44 1509 223923

Abstract

The crystallization of shea stearin was investigated both before and after pre-treatment with silica to remove a small amount (0.7 wt%) of diacylglycerols (DAGs) and oxidized material. NMR (for solid fat content), X-ray diffraction (XRD), polarized light microscopy, confocal Raman microscopy, and non-isothermal, isothermal and “stop-and-return” differential scanning calorimetry (DSC) techniques were used. Four major polymorphs previously found with 1,3-distearoyl-2-oleoyl-sn-glycerol (StOSt) were detected: α, γ, β′, and β; whilst evidence for a further (δ) polymorph was found by DSC and possibly XRD but not Raman spectroscopy. Isothermal crystallization of shea stearins by DSC at 20°C produced α and δ forms within 5 min which then transformed to γ. Microscope images showed that after 1 day these had transformed into β′ with a few crystals of β, with further conversion to β after one week. Silica treated samples showed a faster initial crystallization, with faster transformation or direct crystallization into δ and then γ and β′ forms. Non-isothermal DSC also showed a faster transformation into γ from α on the subsequent remelt. However, further transformation into β appeared to occur at reasonably similar rates for both types, suggesting that DAGs have less influence on this transformation and may be excluded from higher forms.

Practical applications: This paper has two main practical applications: (i) Provides knowledge and understanding of the crystallization and polymorphic behavior of commercial shea stearin, which is a widely used fat in the confectionery, cosmetic, and pharmaceutical industries. (ii) The presence of small amounts of DAGs significantly delays the crystallization process of shea stearin, particularly of the lower polymorphs.

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