Conventional and New Techniques to Monitor Lipid Crystallization

Rigolle, Annelien; Abeele, Koen Van Den; Foubert, Imogen

doi:10.1002/9781118593882.ch17

Cited by 6 publications

(6 citation statements)

References 92 publications

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“…For this, we used the F(0) values obtained from the global fitting analysis and literature values for the density of molten cocoa butter (904 kg/m 3 taken from the thesis of Ladd Parada 45 ) and the density of α-polymorph (978 kg/m 3 taken from Lencki and Craven 46 ). Our SFC value compares well with literature values obtained previously: Marangoni et al 47 (direct quenching), Dewettinck et al 25 (direct quenching), and own pulsed-NMR 45 (stepwise cooling) led to values for the SFC from 9 to 11%, while Rigolle et al 24 estimated the SFC = 5% from wide-angle X-ray scattering (WAXS) data. The lower values from X-ray scattering when compared with the NMR data remain speculative, but it might be explained by the fact that X-ray data are typically recorded faster than NMR data and hence might reflect earlier stages of formation of the α-polymorph.…”

Section: The Form Factor Of the Simple Two-gaussian Model Becomes By Ftsupporting

confidence: 91%

“…An exception concerns the small-angle X-ray scattering (SAXS)-based work of Dewettinck et al, 25 who fitted the diffuse X-ray scattering arising from the liquid state of TAGs with a Lorentzian distribution; however, this was done to only roughly estimate the liquid-to-solid phase ratio in any given diffraction pattern. Structural information in previous publications provides a great deal of information on the crystalline polymorphs, [22][23][24][25]29 but so far, there has not been an integrative approach for simulating the X-ray scattering from TAGs in the transition states.…”

Section: ■ Introductionmentioning

confidence: 99%

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Global Small-Angle X-ray Scattering Data Analysis of Triacylglycerols in the α-Phase (Part II)

Ladd-Parada

Sadeghpour

Vieira³

et al. 2018

J. Phys. Chem. B

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The early stage crystallisation behaviour in a triacylglycerol mixture has been investigated on the nanoscale with a novel global small angle X-ray scattering analysis technique. This method has been tailored for the determination of the electron density profiles (EDP) replicating both, (i) the nanostructural texture of molten TAGs (refer to part I 'Global Small-Angle X-ray Scattering Data Analysis of Triacylglycerols in the Molten State' of this publication series), and (ii) the lamellar structure of the metastable-polymorph. In a first stage, the-phase scattering contribution alone was examined by classical Fourier analysis as well as by globally fitting the data, leading to practically identical EDPs. Based on these findings, we extended our analysis to the entire X-ray scattering contribution arising from molten TAGs and the solid-phase fraction. Remarkably, the experimental and theoretical data agree very well, providing for the first time a detailed nanostructural understanding about the coexisting molecular assemblies. This allowed in turn, also to quantitatively determine the solid fat content (SFC) with X-ray scattering data. Our new theoretical approach for measurement of SFC is based on the global analysis of small angle scattering/diffraction patterns and the SFC-results are in good agreement with values obtained from other techniques such as NMR spectroscopy.

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Section: The Form Factor Of the Simple Two-gaussian Model Becomes By Ftsupporting

confidence: 91%

Section: ■ Introductionmentioning

confidence: 99%

Global Small-Angle X-ray Scattering Data Analysis of Triacylglycerols in the α-Phase (Part II)

Ladd-Parada

Sadeghpour

Vieira³

et al. 2018

J. Phys. Chem. B

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“…The short spacing of a repetition unit between the adjacent hydrocarbon chains of TAG molecules is characterized by the WAXS profile, which defines the sub-cell structure unique to each crystal polymorph. Spacing d is determined as a reciprocal of the magnitude of the scattering vector | s | ( d = 1/| s | = λ /(2sin θ )), where θ is the scattering angle and λ is the wavelength of X-rays applied [ 45 ]. The TAG species and polymorphs of the crystals occurring in the mixtures were identified by comparing the experimental d values with the corresponding values in Table 1 .…”

Section: Resultsmentioning

confidence: 99%

Binary Phase Behavior of 1,3-Distearoyl-2-oleoyl-sn-glycerol (SOS) and Trilaurin (LLL)

et al. 2020

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This paper reports the precise analysis of the eutectic mixing behavior of 1,3-distearoyl-2-oleoyl-sn-glycerol (SOS) and trilaurin (LLL), as a typical model case of the mixture of cocoa butter (CB) and cocoa butter substitute (CBS). SOS was mixed with LLL at several mass fractions of LLL (wLLL); the mixtures obtained were analyzed for polymorphic phase behavior using differential scanning calorimetry (DSC) and synchrotron radiation X-ray diffractometry (SR-XRD). In melt crystallization with constant-rate cooling, SOS and LLL formed eutectics in their metastable polymorphs, allowing the occurrence of a compatible solid solution at wLLL ≥ 0.925. With subsequent heating, the resultant crystals transformed toward more stable polymorphs, then melted in a eutectic manner. For mixtures aged at 25 °C after melt crystallization, eutectics were found in the extended wLLL region, even at wLLL = 0.975. These results indicate that phase separation between SOS and LLL progressed in their solid solution under stabilization. The crystal growth of the separated SOS fraction may cause fat-bloom formation in compound chocolate containing CB and CBS. To solve this problem, the development of retardation techniques against phase separation is expected.

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“…The occurring crystals’ TAG species and polymorphs were identified from the SAXD and WAXD patterns. The long-spacing and short-spacing values for crystal structures were each determined as the reciprocal of the magnitude of the scattering vector | s | (| s | = (2 sin θ)/λ), where θ is the scattering angle and λ is the X-ray wavelength applied …”

Section: Methodsmentioning

confidence: 99%

Interactive Polymorphic Crystallization Behavior in Eutectic Triacylglycerol Mixtures Containing Molecular Compound Crystals

Yoshikawa

Watanabe

Yamamoto

et al. 2022

Crystal Growth & Design

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Polymorphic crystallization behavior in mixture systems of three triacylglycerols (1,3-distearoyl-2-oleoyl-sn-glycerol (SOS), 1,3-dioleoyl-2-stearoyl-sn-glycerol (OSO), and trilauroylglycerol (LLL)) was examined via differential scanning calorimetry (DSC), synchrotron radiation X-ray diffractometry (SR-XRD), and polarized optical microscopy (POM). These three triacylglycerols are widely employed in confections, cosmetics, and other applications. They exhibited immiscible eutectic behavior, in which SOS and OSO formed molecular compound (MCSOS/OSO) crystals with a 1:1 compositional ratio. In each mixture system, the polymorphic form of LLL crystallizing during cooling switched from metastable β′ to stable β soon after crystallization of MCSOS/OSO in the β form. This behavior contrasts strongly with that of a pure system, in which LLL preferentially crystallizes in the β′ form, not directly in the β form. Strong interactions between LLL and MCSOS/OSO may dominate the polymorphic crystallization of LLL even if LLL and MCSOS/OSO do not form a miscible mixture. The present study provides new preparation concepts for novel types of functional fats impervious to structural deterioration during polymorphic transformations from metastable to stable forms.

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Conventional and New Techniques to Monitor Lipid Crystallization

Cited by 6 publications

References 92 publications

Global Small-Angle X-ray Scattering Data Analysis of Triacylglycerols in the α-Phase (Part II)

Global Small-Angle X-ray Scattering Data Analysis of Triacylglycerols in the α-Phase (Part II)

Binary Phase Behavior of 1,3-Distearoyl-2-oleoyl-sn-glycerol (SOS) and Trilaurin (LLL)

Interactive Polymorphic Crystallization Behavior in Eutectic Triacylglycerol Mixtures Containing Molecular Compound Crystals

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