Bert Vanhoutte

Dynamic mathematical model of the crystallization kinetics of fats

A new model able to describe the kinetics of isothermal crystallization is presented: it is a model written in the form of a differential equation allowing use under dynamic temperature variations. It describes the crystallization process as if it is a reversible reaction with a first order forward reaction and a reverse reaction of order n. The model has the advantage of having an analytical solution under isothermal conditions that facilitates parameter estimation. The quality of this model was compared with the more traditional Avrami (with and without induction time) and Gompertz models using different model selection criteria. To show the universality of the model, different fat samples, different crystallization temperatures and different measuring techniques were used for model evaluation. The new model was selected as the best for the majority of the samples and this independent of the model selection criterion used.

The effect of phospholipids and water on the isothermal crystallisation of milk fat

Different amounts of phospholipids (0.00-0.07%) and water (0.00-0.70%) were added to milk fat. The mixtures were crystallised under isothermal conditions and the crystallisation was monitored by differential scanning calorimetry and pulsed nuclear magnetic resonance. The crystallisation behaviour was described with the Avrami and Gompertz model which was fitted by non-linear regression. Variance analysis revealed significant effects, whereas especially the induction time was influenced: higher concentrations of water seemed to decrease the induction time, while higher amount of phospholipids delayed the onset of crystallisation. No interaction effects between phospholipids and water were observed. An attempt to explain the effect of phospholipids on the induction time, based on the molecular interactions between phospholipids and triglycerides is proposed. This principle can be applied for sn-1, 2 diglycerides as well.

Effect of phospholipids on isothermal crystallisation and fractionation of milk fat

Milk fats with different concentrations of water and phospholipids (PL) were crystallised isothermally under static conditions and their crystallisation behaviour was monitored by Differential Scanning calorimetry (DSC) and pulsed nuclear magnetic resonance (pNMR). The Avrami and the Gompertz models, which were fitted by non-linear regression, described the crystallisation process. A significant effect of phospholipid concentration was observed using both techniques (DSC and pNMR). Especially the induction time and the Avrami growth rate constant were altered: higher amounts of PL delayed the onset of static crystallisation. A similar effect of PL on the crystallisation kinetics was observed in a small-scale fractionation. Moreover, the filtration time of the crystal suspension and melting properties of the stearin were strongly affected by the presence of higher concentrations of PL. These observations emphasise the importance of the adequate removal of PL during anhydrous milk fat production.

Development of chromatographic method for the determination of degree of polymerisation of polyglycerols and polyglycerol fatty acid esters

SummaryFrom polyglycerol samples, pure standards of tri and tetraglycerol were obtained using a column chromatographic technique. Polyglycerols were derivatised to trimethyl silyl derivatives to obtain gas chromatographic identification of all linear, branched and cyclic diglycerol isomers and all linear and branched triglycerols. Moreover, quantitative gas chromatographic analysis of the di-, tri- and tetraglycerol content of a polyglycerol sample was developed.Finally a method to characterise, on a quantitative basis, the polyglycerol content of polyglycerol fatty acid esters was developed. It consisted of saponifying the esters, without affecting the degree of polymerisation of the polyglycerols, followed by gas chromatographic analysis of the isolated polyglycerol fraction.

Combined liquid and gas chromatographic characterisation of polyglycerol fatty acid esters

In the present study a combined liquid and gas chromatographic technique is described for the analysis of polyglycerol fatty acid esters. Liquid chromatographic fractionation of samples resulted in pure standards of monoesters of di- and triglycerols and diesters of di- and triglycerols. Confirmation of their identity was achieved by LC-MS analysis. Moreover, a chromatographic identification of the mono- and diesters of cyclic diglycerol was proposed. From the isolation of pure esters and their gas chromatographic analysis, it was revealed that co-elution of several compounds occurred. Thus it was shown that prefractionation of the sample using a simplified liquid chromatographic separation, was necessary in order to characterise the esters correctly. In combination with some other chemical analyses, a complete profile of the chemical composition of polyglycerol fatty acid esters can be obtained.