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21 items found (0 items not approved), displaying 1 to 10.[First/Prev] 1, 2, 3 [Next/Last]

Instruments / Technical Area	Publication Details	Published
B23-Circular Dichroism	Mapping the chiroptical properties of local domains in thin films of chiral silicon phthalocyanines by CD imaging Dora-maria Rasadean , Tiberiu-marius Gianga , Tamas Javorfi , Rohanah Hussain , Giuliano Siligardi , G. Dan Pantos Molecules 25 DOI: 10.3390/molecules25246048 Diamond Proposal Number(s): [23955, 20441, 26447] Open Access Show Abstract ▼ Abstract: The first example of uniformly chiral thin films of silicon phthalocyanines (SiPcs) are reported. The local domains of the films are mapped using circular dichroism (CD) imaging (CDi) technique available at the Diamond B23 beamline. The CDi allowed us to increase the spatial resolution up to 525× when compared with benchtop spectrometers. The results indicate formation on-surface of chiral and stable supramolecular assemblies with homogenous distribution. Chemical functionalization and solvent choice for deposition allow controllable chiroptical properties to be obtained. The method and technique reported in this work could be applied to prepare and characterize a wide variety of chiral thin films.	Dec 2020
I04-1-Macromolecular Crystallography (fixed wavelength)	How to separate kinase inhibition from undesired monoamine oxidase a inhibition—the development of the DYRK1A inhibitor AnnH75 from the alkaloid harmine Anne Wurzlbauer , Katharina Rüben , Ece Gürdal , Apirat Chaikuad , Stefan Knapp , Wolfgang Sippl , Walter Becker , Franz Bracher Molecules 25 DOI: 10.3390/molecules25245962 Open Access Show Abstract ▼ Abstract: The β-carboline alkaloid harmine is a potent DYRK1A inhibitor, but suffers from undesired potent inhibition of MAO-A, which strongly limits its application. We synthesized more than 60 analogues of harmine, either by direct modification of the alkaloid or by de novo synthesis of β-carboline and related scaffolds aimed at learning about structure–activity relationships for inhibition of both DYRK1A and MAO-A, with the ultimate goal of separating desired DYRK1A inhibition from undesired MAO-A inhibition. Based on evidence from published crystal structures of harmine bound to each of these enzymes, we performed systematic structure modifications of harmine yielding DYRK1A-selective inhibitors characterized by small polar substituents at N-9 (which preserve DYRK1A inhibition and eliminate MAO-A inhibition) and beneficial residues at C-1 (methyl or chlorine). The top compound AnnH75 remains a potent DYRK1A inhibitor, and it is devoid of MAO-A inhibition. Its binding mode to DYRK1A was elucidated by crystal structure analysis, and docking experiments provided additional insights for this attractive series of DYRK1A and MAO-A inhibitors.	Dec 2020
B18-Core EXAFS	Understanding the deactivation phenomena of small-pore Mo/H-SSZ-13 during methane dehydroaromatisation Miren Agote-aran , Anna B. Kroner , David S. Wragg , Wojciech A. Sławiński , Martha Briceno , Husn U. Islam , Igor V. Sazanovich , María E. Rivas , Andrew W. J. Smith , Paul Collier , Ines Lezcano-gonzalez , Andrew M. Beale Molecules 25 DOI: 10.3390/molecules25215048 Diamond Proposal Number(s): [11623] Open Access Show Abstract ▼ Abstract: Small pore zeolites have shown great potential in a number of catalytic reactions. While Mo-containing medium pore zeolites have been widely studied for methane dehydroaromatisation (MDA), the use of small pore supports has drawn limited attention due to the fast deactivation of the catalyst. This work investigates the structure of the small pore Mo/H-SSZ-13 during catalyst preparation and reaction by operando X-ray absorption spectroscopy (XAS), in situ synchrotron powder diffraction (SPD), and electron microscopy; then, the results are compared with the medium pore Mo/H-ZSM-5. While SPD suggests that during catalyst preparation, part of the MoOx anchors inside the pores, Mo dispersion and subsequent ion exchange was less effective in the small pore catalyst, resulting in the formation of mesopores and Al2(MOO4)3 particles. Unlike Mo/H-ZSM-5, part of the Mo species in Mo/H-SSZ-13 undergoes full reduction to Mo0 during MDA, whereas characterisation of the spent catalyst indicates that differences also exist in the nature of the formed carbon deposits. Hence, the different Mo speciation and the low performance on small pore zeolites can be attributed to mesopores formation during calcination and the ineffective ion exchange into well dispersed Mo-oxo sites. The results open the scope for the optimisation of synthetic routes to explore the potential of small pore topologies.	Nov 2020
B21-High Throughput SAXS	Design of nanosystems for the delivery of quorum sensing inhibitors: A preliminary study Supandeep Singh Hallan , Paolo Marchetti , Daria Bortolotti , Maddalena Sguizzato , Elisabetta Esposito , Paolo Mariani , Claudio Trapella , Roberta Rizzo , Rita Cortesi Molecules 25 DOI: 10.3390/molecules25235655 Diamond Proposal Number(s): [21035] Open Access Show Abstract ▼ Abstract: Biofilm production is regulated by the Quorum Sensing system. Nowadays, Quorum Sensing represents an appealing target to design new compounds to increase antibiotics effects and avoid development of antibiotics multiresistance. In this research the use of liposomes to target two novel synthetic biofilm inhibitors is presented, focusing on a preformulation study to select a liposome composition for in vitro test. Five different liposome (LP) formulations, composed of phosphatidyl choline, cholesterol and charged surfactant (2:1:1, molar ratio) have been prepared by direct hydration and extrusion. As charged surfactants dicetyl phosphate didecyldimethylammonium chloride, di isobutyl phenoxy ethyl dimethyl benzyl ammonium chloride and stearylamine (SA) and have been used. Liposome charge, size and morphology were investigated by zeta potential, photon correlation spectroscopy, small angle x-ray spectroscopy and electron microscopy. LP-SA was selected for the loading of biofilm inhibitors and subjected to high performance liquid chromatography for entrapment capacity evaluation. LP-SA loaded inhibitors showed a higher diameter (223.6 nm) as compared to unloaded ones (205.7 nm) and a dose-dependent anti-biofilm effect mainly after 48 h of treatment, while free biofilm inhibitors loose activity. In conclusion, our data supported the use of liposomes as a strategy to enhance biofilm inhibitors effect.	Nov 2020
I02-Macromolecular Crystallography I04-Macromolecular Crystallography	Mechanistic insights into the chaperoning of human lysosomal-galactosidase activity: highly functionalized aminocyclopentanes and C-5a-substituted derivatives of 4-epi-isofagomine Patrick Weber , Martin Thonhofer , Summer Averill , Gideon J. Davies , Andres Gonzalez Santana , Philipp Müller , Seyed A. Nasseri , Wendy A. Offen , Bettina M. Pabst , Eduard Paschke , Michael Schalli , Ana Torvisco , Marion Tschernutter , Christina Tysoe , Werner Windischhofer , Stephen G. Withers , Andreas Wolfsgruber , Tanja M. Wrodnigg , Arnold E. Stütz Molecules 25 DOI: 10.3390/molecules25174025 Open Access Show Abstract ▼ Abstract: Glycosidase inhibitors have shown great potential as pharmacological chaperones for lysosomal storage diseases. In light of this, a series of new cyclopentanoid β-galactosidase inhibitors were prepared and their inhibitory and pharmacological chaperoning activities determined and compared with those of lipophilic analogs of the potent β-d-galactosidase inhibitor 4-epi-isofagomine. Structure-activity relationships were investigated by X-ray crystallography as well as by alterations in the cyclopentane moiety such as deoxygenation and replacement by fluorine of a “strategic” hydroxyl group. New compounds have revealed highly promising activities with a range of β-galactosidase-compromised human cell lines and may serve as leads towards new pharmacological chaperones for GM1-gangliosidosis and Morquio B disease.	Sep 2020
B22-Multimode InfraRed imaging And Microspectroscopy	Infrared microspectroscopy and imaging analysis of inflammatory and non-inflammatory breast cancer cells and their GAG secretome Hossam Taha Mohamed , Valerie Untereiner , Gianfelice Cinque , Sherif Abdelaziz Ibrahim , Martin Götte , Nguyet Que Nguyen , Romain Rivet , Ganesh D. Sockalingum , Stephane Brezillon Molecules 25 DOI: 10.3390/molecules25184300 Diamond Proposal Number(s): [15393] Open Access Show Abstract ▼ Abstract: Glycosaminoglycans (GAGs)/proteoglycans (PGs) play a pivotal role in the metastasis of inflammatory breast cancer (IBC). They represent biomarkers and targets in diagnosis and treatment of different cancers including breast cancer. Thus, GAGs/PGs could represent potential prognostic/diagnostic biomarkers for IBC. In the present study, non-IBC MDA-MB-231, MCF7, SKBR3 cells and IBC SUM149 cells, as well as their GAG secretome were analyzed. The latter was measured in toto as dried drops with high-throughput (HT) Fourier Transform InfraRed (FTIR) spectroscopy and imaging. FTIR imaging was also employed to investigate single whole breast cancer cells while synchrotron-FTIR microspectroscopy was used to specifically target their cytoplasms. Data were analyzed by hierarchical cluster analysis and principal components analysis. Results obtained from HT-FTIR analysis of GAG drops showed that the inter-group variability enabled us to delineate between cell types in the GAG absorption range 1350–800 cm−1. Similar results were obtained for FTIR imaging of GAG extracts and fixed single whole cells. Synchrotron-FTIR data from cytoplasms allowed discrimination between non-IBC and IBC. Thus, by using GAG specific region, not only different breast cancer cell lines could be differentiated, but also non-IBC from IBC cells. This could be a potential diagnostic spectral marker for IBC detection useful for patient management.	Sep 2020
B23-Circular Dichroism	The secondary structure of a major wine protein is modified upon interaction with polyphenols Mattia Di Gaspero , Paolo Ruzza , Rohanah Hussain , Claudia Honisch , Barbara Biondi , Giuliano Siligardi , Matteo Marangon , Andrea Curioni , Simone Vincenzi Molecules 25 DOI: 10.3390/molecules25071646 Diamond Proposal Number(s): [14708, 16031] Open Access Show Abstract ▼ Abstract: Polyphenols are an important constituent of wines and they are largely studied due to their antioxidant properties and for their effects on wine quality and stability, which is also related to their capacity to bind to proteins. The effects of some selected polyphenols, including procyanidins B1 and B2, tannic acid, quercetin, and rutin, as well as those of a total white wine procyanidin extract on the conformational properties of the major wine protein VVTL1 (Vitis vinifera Thaumatin-Like-1) were investigated by Synchrotron Radiation Circular Dichroism (SRCD). Results showed that VVTL1 interacts with polyphenols as demonstrated by the changes in the secondary (far-UV) and tertiary (near-UV) structures, which were differently affected by different polyphenols. Additionally, polyphenols modified the two melting temperatures (TM) that were found for VVTL1 (32.2 °C and 53.9 °C for the protein alone). The circular dichroism (CD) spectra in the near-UV region revealed an involvement of the aromatic side-chains of the protein in the interaction with phenolics. The data demonstrate the existence of an interaction between polyphenols and VVTL1, which results in modification of its thermal and UV denaturation pattern. This information can be useful in understanding the behavior of wine proteins in presence of polyphenols, thus giving new insights on the phenomena that are involved in wine stability.	Apr 2020
B21-High Throughput SAXS	Ellagic acid containing nanostructured lipid carriers for topical application: a preliminary study Supandeep Singh Hallan , Maddalena Sguizzato , Gabriella Pavoni , Anna Baldisserotto , Markus Drechsler , Paolo Mariani , Elisabetta Esposito , Rita Cortesi Molecules 25 DOI: 10.3390/molecules25061449 Open Access Show Abstract ▼ Abstract: Ellagic acid (EA) is a potent antioxidant substance of natural origin characterized by poor biopharmaceutical properties and low solubility in water that limit its use. The aim of the present study was to develop lipid-based nanoparticle formulations able to encapsulate EA for dermal delivery. The EA-loaded nanoparticles were prepared using two different lipid compositions, namely tristearin/tricaprylin (NLC-EA1) and tristearin/labrasol (NLC-EA2). The influence of formulations on size, entrapment efficiency, and stability of EA-loaded nanoparticles was investigated. Cryo-TEM and small-angle X-ray scattering (SAXS) analyses showed that no morphological differences are evident among all the types of loaded and unloaded nanostructured lipid carriers (NLCs). The macroscopic aspect of both NLC-EA1 and NLC-EA2 did not change with time. No difference in size was appreciable between empty and drug-containing NLC, thus the nanoparticle diameter was not affected by the presence of EA and in general no variations of the diameters occurred during this time. The entrapment efficiency of both EA-loaded nanoparticles was almost quantitative. In addition, NLC-EA1 maintained EA stability for almost two months, while NLC-EA2 up to 40 days. FRAP (Ferric reducing ability of plasma) assay showed an antioxidant activity around 60% for both the loaded NLC, as compared to the solution. Although both types of NLC are characterized by some toxicity on HaCaT cells, NLC-EA1 are less cytotoxic than NLC-EA2. Taken together these results demonstrated that the inclusion of EA within NLC could improve the water solubility, allowing for a reduction of the dosage. Moreover, both types of NLC-EA maintained a high antioxidant effect and low toxicity.	Mar 2020
I22-Small angle scattering & Diffraction	Non-lamellar liquid crystalline nanocarriers for thymoquinone encapsulation Anan Yaghmur , Boi Vi Tran , Seyed Moein Moghimi Molecules 25 DOI: 10.3390/molecules25010016 Diamond Proposal Number(s): [17191] Open Access Show Abstract ▼ Abstract: Owing to their unique structural features, non-lamellar liquid crystalline nanoparticles comprising cubosomes and hexosomes are attracting increasing attention as versatile investigative drug carriers. Background: Depending on their physiochemical characteristics, drug molecules on entrapment can modulate and reorganize structural features of cubosomes and hexosomes. Therefore, it is important to assess the effect of guest molecules on broader biophysical characteristics of non-lamellar liquid crystalline nanoparticles, since drug-induced architectural, morphological, and size modifications can affect the biological performance of cubosomes and hexosomes. Methods: We report on alterations in morphological, structural, and size characteristics of nanodispersions composed from binary mixtures of glycerol monooleate and vitamin E on thymoquinone (a molecule with wide therapeutic potentials) loading. Results: Thymoquinone loading was associated with a slight increase in the mean hydrodynamic nanoparticle size and led to structural transitions from an internal biphasic feature of coexisting inverse cubic Fd3m and hexagonal (H2) phases to an internal inverse cubic Fd3m phase (micellar cubosomes) or an internal inverse micellar (L2) phase (emulsified microemulsions, EMEs). We further report on the presence of “flower-like” vesicular populations in both native and drug-loaded nanodispersions. Conclusions: These nanodispersions have the potential to accommodate thymoquinone and may be considered as promising platforms for the development of thymoquinone nanomedicines.	Dec 2019
I19-Small Molecule Single Crystal Diffraction	Copper-mediated nitrosation: 2-nitrosophenolato complexes and their use in the synthesis of heterocycles Alexander J. Nicholls , Andrei S. Batsanov , Ian R. Baxendale Molecules 24, 4154 DOI: 10.3390/molecules24224154 Diamond Proposal Number(s): [22240] Open Access Show Abstract ▼ Abstract: A simple protocol yielding ortho-substituted nitrosophenols from phenols is demonstrated, in the form of copper(II) bis(nitrosophenolato) complexes. The developed methodology was applied to a range of substrates, confirming the role of the copper in both the formation and protection of the challenging 1, 2-substitution pattern. Using polymer supported thiourea, the Cu could be stripped from the complexes and thus enabled the isolation or identification of the uncoordinated ligands and their decomposition products, in yields generally low in line with the intrinsic high reactivity of 2-nitrosophenols. The product complexes are useful intermediates as demonstrated in revisiting a formal [4 + 2] cycloaddition with dimethylacetylene dicarboxylate to synthesise bicyclic products in variable yields, revealing the product has a novel structure dierent from those previously reported in the literature.	Nov 2019

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