I22-Small angle scattering & Diffraction
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Diamond Proposal Number(s):
[34844, 37870]
Open Access
Abstract: Fats are essential ingredients widely used in the food industry, as well as in cosmetic and pharmaceutical formulations. Solid fats are complex multicomponent systems primarily composed of triacylglycerols (TAGs), which determine the types and properties of the crystalline structures formed. TAGs crystallize in different polymorphs and stacking configurations, with distinct thermal and mechanical properties that influence the macroscopic structure and sensory profile of fat-based products. In this study, a comprehensive multi-technique analysis of animal-derived fats, specifically chicken and beef fats, was conducted. Chemical characterization was performed and solid fat content (SFC) was determined. Thermal behaviour was investigated using differential scanning calorimetry (DSC), whereas crystallization experiments were conducted using in situ turbidity measurements and synchrotron small-angle and wide-angle x-ray scattering (SAXS/WAXS) for structural characterization. Three different synchrotron experimental setups were used for crystallization experiments, including static and sheared conditions. The results demonstrate that the crystallization behaviour of beef and chicken fat samples closely correlate with their TAGs composition. Synchrotron x-ray scattering provided structural insights, highlighting how the polymorphic behaviour is influenced by fat origin and crystallization conditions. For both animal fat types, all three main polymorphs and possible transitions were detected. Moreover, the presence of shear promoted crystallization of stable polymorphs.
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May 2026
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I22-Small angle scattering & Diffraction
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Diamond Proposal Number(s):
[39895]
Open Access
Abstract: Benchtop ultra-small-angle X-ray scattering (USAXS) offers a practical route to probing micron-scale structural features in soft-matter systems, provided that instrumental limitations are explicitly defined and respected. In this work, a Rigaku NANOPIX mini USAXS instrument is used to characterize hierarchical fat crystal networks, with emphasis on establishing a reliable analysis window and appropriate treatment of slit-geometry effects. Analyzer crystal rocking curves are employed to define a lower bound for quantitative analysis (qmin ≈ 3.4 × 10−4 Å−1), while counting-statistics considerations define an upper bound (qmax ≈ 1.4 × 10−2 Å−1). Data outside this window are shown to be strongly influenced by direct-beam and noise artifacts and are therefore excluded from interpretation. Within the valid q-range, slit-smearing effects inherent to Bonse–Hart geometries are addressed by smearing structural models using open-source SASView software rather than numerically desmearing experimental data. Using cocoa butter, commercial chocolate, and a reference triglyceride mixture as representative case studies, power-law scattering regimes are extracted and compared with synchrotron SAXS measurements over overlapping q-ranges. While absolute slope values vary between instruments and samples, benchtop USAXS captures consistent scattering trends, including stable power-law behavior in tempered systems and transient curvature in untempered samples that diminishes upon storage. These results demonstrate that benchtop USAXS, when interpreted within a rigorously defined q-window and with appropriate resolution treatment, provides a reproducible and accessible tool for comparative analysis of hierarchical fat systems. More broadly, this study outlines best practices and interpretive boundaries for laboratory-scale USAXS measurements in soft-matter research.
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Mar 2026
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I22-Small angle scattering & Diffraction
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Diamond Proposal Number(s):
[39895]
Abstract: A hierarchical additive framework is developed for the quantitative interpretation of X-ray scattering (SAXS) from lamellar crystalline materials. The formulation extends the classical decomposition I(q) = P(q)S(q), with I(q) the scattering intensity, P(q) the form factor, and S(q) the structure factor, by explicitly coupling the contributions of three structural regimes: low-q power-law (fractal-like) aggregation, intermediate-q Guinier curvature arising from finite nanocrystal dimensions, and high-q Bragg reflections associated with lamellar periodicity. Each regime is expressed analytically and linked through shared structural parameters, ensuring physical consistency across length scales. The scattering intensity is interpreted as the Fourier transform of the electron-density correlation function, following Debye’s original formulation (Debye, 1915), which naturally accommodates cross-correlations between internal morphology and interparticle organization. Simulated scattering profiles illustrate how parameter variations influence the overall signature, and the model is applied to synchrotron SAXS data from cocoa-butter triacylglycerols to demonstrate practical fitting performance. The resulting approach provides a compact and physically rigorous description of hierarchical lamellar systems and offers a generalizable framework for complex materials in which form and structure factors cannot be treated independently.
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Mar 2026
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I22-Small angle scattering & Diffraction
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Diamond Proposal Number(s):
[34844, 37870]
Open Access
Abstract: Efficient food resources management, particularly through minimization of waste across the production and supply chain, is essential for creating a resilient, circular agri-food system. The rice industry is one of the largest sectors in agri-food, supporting over half of the global population. This work focuses on valorizing the lipidic fraction of rice bran, a major by-product of rice processing, to contribute to reducing the environmental impact of rice production. Novel purification processes of rice bran wax (RBX) from rice bran are presented, together with their environmental impact assessment. Rice bran butter (RBB) was initially extracted using supercritical CO2, followed by the separation of its main components, rice bran oil (RBO) and rice bran wax (RBX), through combinations of different physical unit operations including crystallization, centrifugation, solvent extraction and filtration. The purification strategies developed involved green solvents such as ethanol and isopropanol, compared to the commonly used hexane. The purified products were characterized in terms of their chemical properties via chromatographic techniques. Differential Scanning Calorimetry (DSC) and X-ray diffraction were used to determine structural and thermal properties of the material extracted. A Life Cycle Assessment (LCA) was also conducted to determine the environmental impact of the designed extraction and separation processes. The LCA highlighted that the optimal process configuration balances wax extraction yield, energy consumption, and solvent use. Process #2 using ethanol emerged as the most sustainable option, achieving the highest performance with the lowest environmental impact.
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Dec 2025
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I18-Microfocus Spectroscopy
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Diamond Proposal Number(s):
[34311]
Abstract: Rice is a staple food for over half the world's population. This study uniquely investigates the spatial distribution of key micronutrients (Cu, Mn, Fe, Zn) in cooked brown, white, and parboiled rice using Synchrotron Micro-X-ray Fluorescence (sXRF) for the first time. Complementary analysis with Inductively Coupled Plasma Mass Spectrometry (ICP-MS) validates bulk elemental concentrations. Results from this dual-approach study reveal significantly higher micronutrient concentrations in brown rice compared to white or parboiled rice, with nutrients predominantly localised in the peripheral layers and minimal presence in the endosperm. Notably, sXRF imaging identified nutrient-rich pockets within the grain periphery, offering new perspectives on nutrient distribution beyond peripheral accumulation. Additional insights include the impact of rice section thickness (50 and 150 μm) and beam dwell times (0.5 and 30s) on sXRF sensitivity and resolution, highlighting trade-offs in detection capabilities, advancing our understanding of micronutrient localisation in cooked rice.
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Dec 2025
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B21-High Throughput SAXS
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Diamond Proposal Number(s):
[28976]
Abstract: Structural characterization of commercially available gluten-free pasta is achieved here by combining small-angle x-ray and neutron scattering with contrast variation, and compared to the analogous regular gluten-containing pasta variety. In particular, the use of neutron and contrast variation allowed us to isolate the information about the gluten matrix and the starch granules. The broad peak that reflects the structure of the starches is lost as a function of cooking. This effect is more dramatic for the gluten-free pasta, indicating that the absence of gluten strongly promotes the gelation of the starches. Furthermore, the presence of salt in the cooking water is found to preserve the structural properties of the pasta, while at the same time it promotes the degradation of the starch granules. This study is the first step for a structural characterization of commercially-available pasta, moving forward the classic model system used so far to achieve information on the relation between pasta microstructure and its digestibility.
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Aug 2025
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I22-Small angle scattering & Diffraction
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Diamond Proposal Number(s):
[29532]
Open Access
Abstract: Ultrasound standing waves (USW) produce a force capable of displacing micrometer-sized free-flowing particles in a fluid, wherein this phenomenon is also referred to as acoustophoresis. However, the effect of acoustophoresis on dynamically changing and growing crystal networks is unclear. An example of such a system are monoglyceride (MG)-based oleogels, which are free-flowing lipids (e.g., vegetable oils) structured with a lipid-crystal network. In this work, we use MG oleogels as an example system to investigate the acoustophoretic effect on the structuration of a growing crystal network. For this purpose, multifaceted characterization is conducted utilizing optical and coded excitation scanning acoustic microscopy as well as small-angle X-ray scattering, respectively. The optical microscopy results show that USW produces local density differences of the structuring crystalline material and induces the orientation of the MG platelets. X-ray diffraction measurements confirm these findings and show a 23% average increase in MG platelet correlation length, which can be linked to platelet thickness, as well as an increase in the MG nanoplatelet surface smoothness. These findings produce a foundation for better understanding the effect of acoustophoresis in dynamically developing lipid-based materials and illuminate the mechanical changes that arise because of USW treatment.
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Jun 2025
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I03-Macromolecular Crystallography
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Diamond Proposal Number(s):
[21625]
Open Access
Abstract: Listeria monocytogenes is a ubiquitous, psychrotrophic human pathogen that can cause listeriosis, a serious illness for vulnerable populations. Some foods, such as Hispanic-style fresh cheeses like queso fresco, pose a specific risk because there are no widely accepted or available methods for L. monocytogenes mitigation that are both effective and able to maintain the properties of the products. Listeria-specific bacteriophages encode endolysins that are able to cleave the peptidoglycan layer of L. monocytogenes cells externally, showing promise as a potential solution to this problem. PlyP100, from the GRAS Listeria phage P100, is one such endolysin that can prevent the growth of L. monocytogenes in both lab culture conditions and a miniaturized queso fresco model. In this work, we aimed to understand the structural and functional properties of PlyP100. An AlphaFold prediction suggested the presence of three separate domains (D1, D2, and D3). By solving a crystal structure of D1 and assessing various domain truncations, we present evidence that D1 is responsible for catalytic activity, D3 is sufficient for cell wall binding, and D2 is necessary for full function of the enzyme against live cells. Additionally, we performed point mutations in D1 and compared PlyP100 to proteins with similar structures, including S. pneumoniae LytA and Listeria endolysin Ply511, in order to understand its specific enzymatic mechanism and target strain specificity. These insights into the structure and function of PlyP100 will aid future work aiming to engineer better endolysins as safe food antimicrobials.
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May 2025
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I03-Macromolecular Crystallography
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Diamond Proposal Number(s):
[12346]
Abstract: This study explores the endo-levanase from Bacillus licheniformis (LevB1), providing new insights into how this enzyme selectively hydrolyzes levan chains. By analyzing the first resolved crystal structure of LevB1, conducting detailed simulations, and comparing it to other endo- and exo-fructanases, we identified key factors underlying its specificity. Experiments designed to explore this specificity revealed the critical role of three minus and three plus subsites in determining the enzyme’s endo-specificity. We identified six specific subsites essential for the enzyme’s ability to cleave levan chains at random internal linkages (endo-specificity) rather than at defined fructosyl nonreducing ends (exo-specificity). This research underscores the importance of enzyme–fructan interaction stability during the catalytic reaction in this process, highlighting the need for dynamic modeling to fully capture enzyme specificity, as conventional docking alone cannot fully explain the stability and motion of carbohydrate chains in the catalytic site. These findings contribute to a deeper understanding of the factors that influence endo- and exo-cleavage specificity in levan and inulin polymers, with broader implications for fructan metabolism and, eventually, the industrial production of fructose and/or fructo-oligosaccharides.
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Apr 2025
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I22-Small angle scattering & Diffraction
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Diamond Proposal Number(s):
[34844]
Open Access
Abstract: Due to the increasing global demand for chocolate products and changes in consumer preferences, chocolate manufacturers have recently started to explore novel solutions to reformulate chocolate. Milk fat alternatives (MFA) are blends of triglycerides from different plant-based sources that resemble anhydrous milk fat in physical properties, particularly thermal behavior and solid fat content. However, in order to use MFA as potential ingredients for vegan milk chocolate formulations, it is necessary to understand their crystallization behavior, particularly in light of their chemical composition. Here, we applied synchrotron X-ray scattering, polarized light microscopy, and differential scanning calorimetry to investigate the crystallization behavior of four selected commercial MFAs (MF1, 2, 3, and 4), on their own and mixed with cocoa butter (CB). Chemical characterization revealed significant differences among samples and with both anhydrous milk fat (MF) and CB. POP-rich MF1 presented a specific polymorphic and thermal behavior, with the unstable β′ form persisting for longer times than all other samples. Sample MF2 exhibited a polymorphic behavior more similar to CB in terms of number, type, and melting behavior due to the compositional similarities (e.g., prevalence of both SOS and POP). SOS-rich MF3 was characterized by metastable forms γ and β′(3L), whereas MF4 at ambient conditions showed only β(2L) forms due to its specific composition. Mixtures of CB and all MFAs behaved similarly to CB and MF mixtures, with good miscibility at ambient temperature and a lower melting point. Despite significant differences in chemical composition, MF4 presented similar solid fat content compared to MF; this is due to the high amount of relatively long chain, unsaturated fatty acids and the broad distribution of different TAGs, which all lower the melting point of this sample.
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Apr 2025
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