Characterisation of Fat Crystal Polymorphism in Cocoa Butter by Time-Domain NMR and DSC Deconvolution

The polymorphic state of edible fats is an important quality parameter in fat research as well as in industrial applications. Nowadays, X-ray diffraction (XRD) is the most commonly used method to determine the polymorphic state. However, quantification of the different polymorphic forms present in a sample is not straightforward. Differential Scanning Calorimetry (DSC) is another method which provides information about fat crystallization processes: the different peaks in the DSC spectrum can be coupled to the melting/crystallisation of certain polymorphs. During the last decade, nuclear magnetic resonance (NMR) has been proposed as a method to determine, qualitatively and/or quantitatively, the polymorphic forms present in fat samples. In this work, DSC- and NMR-deconvolution methods were evaluated on their ability to determine the polymorphic state of cocoa butter, with XRD as a reference method. Cocoa butter was subjected to two different temperature profiles, which enforced cocoa butter crystallization in different polymorphic forms. It was found that XRD remains the best method to qualitatively determine the polymorphic state of the fat. Whereas the quantitative NMR and DSC deconvolution results were not fully in line with the XRD results in all cases, NMR deconvolution showed great promise both in a qualitative and quantitative way.

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Differentiated Scanning Calorimetry of Model Systems with Cocoa Butter

Food Industry ◽

10.29141/2500-1922-2020-5-2-4 ◽

2020 ◽

Vol 5 (2) ◽

pp. 29-36

Author(s):

Alexander Vereshchagin ◽

Irina Reznichenko ◽

Nikolay Bychin

Keyword(s):

Cocoa Butter ◽

Palm Olein ◽

Palm Stearin ◽

Model Systems ◽

Scanning Calorimetry ◽

Glucose Syrup ◽

Polymorphic Modifications ◽

Confectionery Products ◽

System Temperature ◽

Dsc Method

The article concerns the research specificity of model systems such as cocoa butter – palm olein, cocoa butter – sucrose and cocoa butter – glucose syrup by the differential scanning calorimetry (DSC) method. The researchers run experiments in the temperature range from –100 to –50°C at a heating rate of 10 °C/min. In the cacao butter – palm olein system an eutectic occurs with a palm olein content of 30.0 % indicating the limited solubility of palm olein in cocoa butter. In the cocoa butter – sucrose system, cocoa butter crystallizes as in the α-form (10,0– 30,0; 60.0–90.0 % MK), and as a mixture of α-and β-forms of MK (40.0; 50,0; 70,0 and 80.0 %). Sucrose stabilizes low-temperature polymorphic modifications of cocoa butter. In the cocoa butter – glucose syrup system, temperature of samples melting is 21-22 °C. This composition is promising for use as a filling of confectionery products and glazes production. In this regard, a man can use glucose syrup only in the candy cases production. The role of surfactants used for the formation and stabilization of cocoa butter polymorphs and increasing the thermal stability of the shock-lad without the introduction of palm stearin requires separate consideration.

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Formation of Pharmaceutical Salts and Cocrystals via Vapour-Assisted Tumbling (VAT) – A Solvent Efficient Process with Potential Industrial Applications

10.33774/chemrxiv-2021-qgnfh-v2 ◽

2021 ◽

Author(s):

Alexander J. Stirk ◽

Fabio E. S. Souza ◽

Jenny Gerster ◽

Fatemeh M. Mir ◽

Avedis Karadeolian ◽

...

Keyword(s):

Differential Scanning Calorimetry ◽

Environmental Impact ◽

Industrial Applications ◽

X Ray Diffraction ◽

Scanning Calorimetry ◽

New Techniques ◽

X Ray ◽

Industry Standard ◽

Pharmaceutical Salts ◽

Solid Form

Crystallisations on both the academic and industrial scale often use large volumes of solvent. In order decrease the environmental impact of such processes, new techniques must be discovered that increase the efficiency of the solvents used. Introduced here is a process that combines repurposed industry standard hardware and aspects of mechanochemistry to produce a technique we call “Vapour Assisted Tumbling” (VAT). Pharmaceutical and well-known cocrystals and salts were formed by tumbling the coformers in an atmosphere of vaporised solvent, in this study, methanol (MeOH). This was done inside a custom built analogue of an industrial rotary cone dryer (RCD). It was found that a desired solid form could be obtained as monitored by powder X-ray diffraction and differential scanning calorimetry. By repurposing industrial RCDs, it is feasible that solid forms can be crystallised with both minimal and reusable/recyclable solvent – drastically lowering the environmental impact of such transformations.

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Kokum Butter: Potential Source of in Confectionary Industry

Journal of Scientific Research and Reports ◽

10.9734/jsrr/2021/v27i1130463 ◽

2021 ◽

pp. 120-128

Author(s):

S. B. Kalse ◽

A. A. Sawant ◽

S. B. Swami

Keyword(s):

Fatty Acid Composition ◽

Cocoa Butter ◽

Poor Quality ◽

Industrial Applications ◽

Extraction Techniques ◽

Important Ingredient ◽

Processing Industry ◽

Potential Source ◽

Increasing Demand

Cocoa butter is an important ingredient in the confectionery industry because of its unique physicochemical properties which are given by its peculiar fatty acid composition. Increasing demand and shortage of supply for cocoa butter, poor quality of individual harvests, economic advantages, and some technological benefits have induced for the development of its alternative or replacer. Kokum kernel is a byproduct of the agro-processing industry in India containing about 40–50 % fat which has the potential as a worthy cocoa butter alternative (CBA). However, inefficient extraction techniques that are practiced at the cottage level restrict its industrial applications.

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Synthesis and thermal properties of some phenolic resins

Innovaciencia Facultad de Ciencias Exactas Físicas y Naturales ◽

10.15649/2346075x.508 ◽

2019 ◽

Vol 7 (1) ◽

pp. 1-15

Author(s):

Alshawi F M ◽

Abdul Razzq K ◽

Hanoosh W S

Keyword(s):

Phenol Formaldehyde ◽

Chemical Properties ◽

Decomposition Temperature ◽

Industrial Applications ◽

Stability Study ◽

Curing Temperature ◽

Molar Ratio ◽

Scanning Calorimetry ◽

Phenolic Resins ◽

Physical And Chemical

Introduction: Phenolic resins have been in use since the early twentieth century and are considered the first class of synthetic polymers to achieve commercial success, moreover phenolic resins continue to succeed and attract special interest in a large range of industrial applications such as adhesives, paints, and composites; because of their unique physical and chemical properties. Materials and Methods: Prepolymers resol resins (RR, RH, RP, and RC) were synthesized by the reaction of phenolic compounds (resorcinol, hydroquinone, phloroglucinol, and catechol) respectively, with formaldehyde at molar ratio phenol/ formaldehyde 1/1.5, using sodium hydroxide as a catalyst. These resins were characterized by FTIR. The curing reaction of these resins was evaluated using differential scanning calorimetry (DSC), while the thermal stability study was evaluated using thermogravimetric analysis (TGA). Results and Discussion:From the results showing that these prepolymers have different curing temperatures and curing energy, while the TGA study showed that the cured resins have decomposition temperature more than 300 ºC, and char residue at 650 ºC more than 60%. Conclusions: These resol resins have different gel times (8-55) min, and viscosities (435-350) mpa.s. The curing temperature of these resin obtained from DSC curves was (120, 129, 105 and 127 °C), while the thermal behavior of the cured resins obtained from TGA curves showed that these cured resin have two decomposition temperatures and the rate of decomposition in the order of RC < RR< .

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ATR-IR coupled to partial least squares regression (PLSR) for monitoring an encapsulated active molecule in complex semi-solid formulations

The Analyst ◽

10.1039/c8an00547h ◽

2018 ◽

Vol 143 (10) ◽

pp. 2377-2389 ◽

Cited By ~ 1

Author(s):

Lynda Miloudi ◽

Franck Bonnier ◽

Kevin Barreau ◽

Dominique Bertrand ◽

Xavier Perse ◽

...

Keyword(s):

Partial Least Squares Regression ◽

Industrial Applications ◽

Attenuated Total Reflectance ◽

Great Promise ◽

Least Squares Regression ◽

Active Molecule ◽

Total Reflectance ◽

Quality Control Tool ◽

Semi Solid ◽

Control Tool

Attenuated Total Reflectance-Infrared (ATR-IR) spectroscopy holds great promise for industrial applications as a quality control tool for complex galenic formulations.

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Molecular Origins of Polymorphism in Cocoa Butter

Annual Review of Food Science and Technology ◽

10.1146/annurev-food-070620-022551 ◽

2021 ◽

Vol 12 (1) ◽

Author(s):

Saeed M. Ghazani ◽

Alejandro G. Marangoni

Keyword(s):

Cocoa Butter ◽

Ternary Phase ◽

Annual Review ◽

Food Science ◽

Publication Date ◽

Polymorphic Transformations ◽

Crystal Forms ◽

Polymorphic Forms ◽

Phase Behaviors ◽

Metastable Forms

Cocoa butter displays complex crystallization behavior and six crystal polymorphic forms. Although the crystal structure of cocoa butter has been studied extensively, the molecular interactions between cocoa butter triacylglycerols in relation to polymorphic transformations from metastable forms (forms III and IV) to stable crystal forms (forms V and VI) remain largely unknown. In this review, the triclinic polymorphism and melting profiles of the major triacylglycerols in cocoa butter—POP, POS, and SOS—are reviewed, and their binary and ternary phase behaviors in metastable (pseudoβ′) and stable (β2) crystal forms are discussed. We also attempt to clarify how the transformation of cocoa butter from form IV to V, as a critical step in the tempering of chocolate, is controlled by POS interactions with both POP and SOS. Moreover, we show how the crystal forms V and VI of cocoa butter are templated by crystal forms β3 and β1 of POS, respectively. Expected final online publication date for the Annual Review of Food Science and Technology, Volume 12 is March 2021. Please see http://www.annualreviews.org/page/journal/pubdates for revised estimates.

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Self-repairing mechanism and surface characterization of compressor vanes lubricated with oil added with magnesium silicate hydroxide nanorods

Manufacturing Review ◽

10.1051/mfreview/2019025 ◽

2019 ◽

Vol 6 ◽

pp. 26

Author(s):

Libo Wang ◽

Yi Yang ◽

Yi Qin ◽

Gang Yang ◽

Yuan Qin ◽

...

Keyword(s):

Surface Characterization ◽

Friction And Wear ◽

Magnesium Silicate ◽

Composite Membranes ◽

Great Depth ◽

Industrial Applications ◽

The Self ◽

Great Promise ◽

Surface Modified

Using magnesium silicate hydroxide as additive of lubricating oils for reducing friction in engineering equipment/machinery has been researched intensively. However, some mechanism relating to the growth of the self-repairing layers on the won surfaces is still not clearly explained. At the same time, using magnesium silicate hydroxide (MSH) in the form of nanorods showed great promise in reducing friction and wear. In this study, surface-modified MSH in the form of nanorods was used as additive of polyolester oil (POE) which was then used for the lubrication of compressor vanes. The sample parts were studied on the morphology and the microstructure of the self-repairing layer in a great depth. The results showed that self-repairing layers with different thicknesses were generated on the worn surfaces when the POE with 1 wt.% nanorods-MSH was used. It was found that the self-repairing layers consist of organic–inorganic composite membranes, and with increase of working time of the compressor vanes, the self-repairing layers become denser and thicker, while their micro-structural form remains to be similar. The situ-repairing capability of the metal surfaces (roller-vane pair of the compressor) enforced by the MSH nanorods is very significant, indicating high potential for industrial applications where boundary and mixed lubrications are needed.

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Effect of Dual Modification on the Spectroscopic, Calorimetric, Viscosimetric and Morphological Characteristics of Corn Starch

Polymers ◽

10.3390/polym11020333 ◽

2019 ◽

Vol 11 (2) ◽

pp. 333 ◽

Cited By ~ 9

Author(s):

Ulin Basilio-Cortés ◽

Leopoldo González-Cruz ◽

Gonzalo Velazquez ◽

Gerardo Teniente-Martínez ◽

Carlos Gómez-Aldapa ◽

...

Keyword(s):

Acid Hydrolysis ◽

Short Range ◽

Corn Starch ◽

Morphological Characteristics ◽

Industrial Applications ◽

Peak Time ◽

Starch Granules ◽

Scanning Calorimetry ◽

Pasting Temperature ◽

Ftir And Raman Spectroscopy

The effect of dual modification of corn starch, including hydrolysis and succinylation, were evaluated through peak viscosity (PV) analysis, differential scanning calorimetry (DSC), scanning electron microscopy (SEM), Fourier transform infrared spectroscopy (FTIR) and Raman spectroscopy. This dual modification was shown to increase the reaction efficiency (RE) and degree substitution (DS) compared with starches that were not subjected to acid hydrolysis pretreatment with a 44% and 45% increase respectively. After acid hydrolysis pretreatment, the surface of the corn starch granules exhibited exo-erosion and whitish points due to the accumulation of succinyl groups. The peak viscosity was reduced significantly with the acid hydrolysis pretreatment (between 3 and 3.5-fold decrease), which decreased the pasting temperature and peak time to 20 °C and 100 s respectively. In addition, the dual modification of corn starch altered certain thermal properties, including a reduction in the enthalpy of gelatinization (ΔH) and a higher range of gelatinization (around 6 °C), which may effectively improve industrial applications. Modifications on the FTIR spectra indicated that the dual modification affected the starch crystallinity, while the Raman spectra revealed that the dual modification disrupted the short-range molecular order in the starch. Rearrangement and molecular destabilization of the starch components promoted their granular amphiphilic properties.

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Development of an Expanded Snack of Rice Starch Enriched with Amaranth by Extrusion Process

Molecules ◽

10.3390/molecules24132430 ◽

2019 ◽

Vol 24 (13) ◽

pp. 2430 ◽

Cited By ~ 3

Author(s):

Lilisbet Castellanos-Gallo ◽

Tomás Galicia-García ◽

Iván Estrada-Moreno ◽

Mónica Mendoza-Duarte ◽

Rubén Márquez-Meléndez ◽

...

Keyword(s):

Reference Method ◽

Thermal Characterization ◽

Extrusion Process ◽

Raw Material ◽

Rice Starch ◽

Scanning Calorimetry ◽

Clear Trend ◽

Substitution Degree ◽

Ft Ir ◽

Rice Milling

This study aimed to obtain a second-generation snack by extrusion from the by-product of rice milling enriched with amaranth. The raw material used was amaranth flour (AF), rice starch (NS) and modified rice starch (MS), which were evaluated by the analysis of substitution degree (SD), differential scanning calorimetry (DSC), viscosity (RVA), Fourier transform infrared spectroscopy (FT-IR) and X-ray diffraction (XRD). The snacks were expanded by extrusion and microwave oven, as a reference method. The samples were evaluated in hardness (D), expansion index (EI), apparent density (DAP), and protein content (P). Afterward, the optimized samples were evaluated by scanning electron microscopy (SEM) and resistant starch (RS). During the thermal characterization, a clear trend in the decrement in gelatinization temperatures was observed (78.35 to 63.90 °C in NS and MS respectively). The curves obtained in RVA analyses showed typical behavior of native (6.35 Pa.s) and extruded starches (2.88 Pa.s), with a significant decrease in viscosity peak. Through the analysis of FT-IR, the introduction of the functional acetyl group (stretching at a wavelength of 1735 cm−1) was corroborated. Snack samples results showed a maximum hardness in MS, with a value of 121 N, and the NS (100%) presented the highest EI value (1.41). The lowest DAP values were obtained for the MS (0.48 g/cm3, 100%) and AF (0.49 g/cm3, 100%) samples. P increased to a higher concentration of AF. In the optimum formulation, the SEM image showed that the expanded microwave sample increased the porosity and obtained an RS value of 8.2%. The formulation obtained in the present study presents high characteristics to be used in the development of a healthy snack.

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