X-ray Powder Diffraction Analysis Research Articles

Improving oral delivery of ciprofloxacin through in situ spray drying and acid counterions

This study explores the application of a novel three-fluid nozzle spray drying technique in formulating in situ ciprofloxacin (CFX) salts for improved oral drug delivery. The used key materials in the study include CFX combined with four different counterions: succinic acid (SA), glutaric acid (GA), adipic acid (AA), and pimelic acid (PA), alongside hydroxypropyl methylcellulose (HPMC) as a matrix agent. The process utilized a three-fluid nozzle spray drying technique to produce CFX salts directly with these acids during the process, creating three types of formulations: pure salts (SALT), solutions of drug and polymer (SOL), and nanoprecipitates of drug within a polymer matrix (SUS). Powder X-ray Diffraction (PXRD) and Scanning Electron Microscopy (SEM) analyses revealed that the formulations predominantly exhibited an amorphous structure with varied particle shapes and sizes. The dissolution profiles of CFX salts show a marked burst release within the initial 5 min, with CFX-GA leading at nearly double the release rate of CFX-AA, after which all formulations rapidly achieve over 90 % dissolution and maintain a stable release up to 30 min. This pattern was attributed to the interactions between the drug salts and HPMC, resulting in a sustained release of CFX. In vivo experiments with rabbits revealed a higher plasma concentration of CFX for CGAH-sus compared to CGAH-sol, highlighting the enhanced bioavailability of the SUS formulation. The amorphous nature of CGAH-sus, with ionization confirmed through Raman spectroscopy, facilitated efficient drug release and absorption in the gastrointestinal tract. This study illustrates the effectiveness of the three-fluid nozzle spray drying method in producing salts with varied physical properties and dissolution profiles, holding potential for advanced oral drug delivery systems.

Lanthanide-based F-MOFs: Structure, hydrolytic stability, spectral and magnetic properties

A series of five novel lanthanide-based fluorinated metal-organic frameworks (Ln-F-MOFs) have been synthesized under solvothermal conditions by the reaction of 3,3′-bis(trifluoromethyl)-[1,1′-biphenyl]-4,4′-dicarboxylic acid (H2L) and lanthanide Ln(III) ions (Ln(III)La, Ce, Pr, Nd and Eu). Powder X-ray diffraction (PXRD) analysis revealed that all prepared complexes are isostructural. A single-crystal X-ray crystallographic study of one representative of the isostructural group, namely {[La2(L)3(DMF)2(H2O)2]}n showed, that compound crystallizes in a triclinic system with space group P-1. The lattice parameter values are a = 8.563(2) Å, b = 13.199(3) Å, c = 16.008(4) Å, α = 104.588(7) °, β = 92.904(7) ° and γ = 92.717(7) °, with two formula units in the unit cell. The overall structure is formed by 2D polymeric layers, which are arranged into a semi-3D supramolecular structure through hydrogen bonds and other intramolecular interactions. The study of the hydrophobic properties of the complexes showed that the complexes exhibit surface hydrophobicity with a “rose petal effect” and a contact angle of approximately 107°. However, the structures are not hydrolytically stable in the long term and the structure starts to delaminate after two days in water. This is a manifestation of the fact that the complexes do not form a 3D polymer network, it is made up of 2D layers connected only by weak non-bonding interactions. The photoluminescence properties of the Ln(III) complexes are determined by the characteristic 5d-4f or 4f-4f electron transitions for the individual lanthanide ions. The magnetic properties of Nd(III), Pr(III) and Eu(III) variants were studied. The magnetic properties of {[Pr2(L)3(DMF)2(H2O)2]}n are characterized by the presence of a low-lying quasi-doublet with 15.6 cm−1 energy splitting, whereas Eu(III) variant is nonmagnetic at low temperatures, but the magnetic 7F1 state is accessible by thermal excitation. For Nd(III) complex, the X-band EPR measurements were performed. Since 1D channels with dimensions of 4.90 × 7.23 Å2 are present within the structure, the adsorption of N2, CO2 and H2 gases was also studied.

Palmitic acid-mediated modulation of crystallization dynamics in amylose microparticle formation: From spherical to macaron and disc shapes

Here, we investigated the complexation of short chain amylose (SCAs) and palmitic acid (PA), serving as polymeric building blocks that alter the selectivity and directionality of particle growth. This alteration affects the shape anisotropy of the particles, broadening their applications due to the increased surface area. By modifying the concentration of PA, we were able to make spherical, macaron, and disc-shaped particles, demonstrating that PA acts as a structure-directing agent. We further illustrated the lateral and longitudinal stacking kinetics between PA-SCA inclusion complexes during self-assembly, leading to anisotropy. Transmission electron microscope (TEM) and scanning electron microscope (SEM) revealed the structural difference between the initial and final morphologies of palmitic acid-short chain amylose particles (PA-SCAPs) compared to those of short-chain amylose particle (SCAPs). The presence of PA-SCA inclusion complex in the anisotropic particles was confirmed using nuclear magnetic resonance (NMR) and powder x-ray diffraction (XRD) analysis.

CRYSTALLO-CO-AGGLOMERATION OF SIMVASTATIN: IMPROVING DISSOLUTION AND MICROMERITIC PROPERTIES

Simvastatin (SMV), a poorly soluble drug, faces challenges in pharmaceutical formulation due to its limited solubility and poor flow properties. This study aimed to enhance the physicochemical properties of SMV by preparing spherical crystals using a crystallo-co-agglomeration. Spherical crystals of SMV were prepared by dissolving the drug in methanol and adding it to an aqueous solution containing PVP K-30 and PEG 6000 under constant stirring. The resulting agglomerates were filtered, dried, and characterized using Fourier Transform Infrared (FTIR) spectroscopy, Powder X-Ray Diffraction (PXRD), Differential Scanning Calorimetry (DSC), Scanning Electron Microscopy (SEM), and dissolution testing. Micromeritic properties, including bulk density, Hausner ratio, compressibility index, angle of repose, and flowability, were also evaluated. FTIR confirmed the chemical integrity of SMV with minor shifts indicating interactions with stabilizers. PXRD and DSC analyses revealed reduced crystallinity and partial amorphization in the spherical crystals. SEM showed spherical morphology. Dissolution testing demonstrated a significantly enhanced dissolution rate for the spherical crystals compared to pure SMV. Improved micromeritic properties were also observed, indicating better flowability and packing density. Spherical crystallization significantly improved the solubility, dissolution rate, and flowability of SMV. This technique offers a promising strategy for enhancing the bioavailability and pharmaceutical performance of poorly soluble drugs.

Extraction and characterization of biocompatible hydroxyapatite (Hap) from red big eye fish bone: Potential for biomedical applications and reducing biowastes

In this study, nanostructured hydroxyapatite (HAp) was successfully extracted from the bones of Priacanthus macracanthus (Red Big Eye), a species commonly processed in the fish industry, generating significant waste. The extraction process utilized an alkaline hydrolysis method optimized with 2 M sodium hydroxide at 250 °C for 5 h, producing high-purity HAp. Fourier transform infrared spectroscopy (FT-IR) confirmed the presence of characteristic phosphate peaks at 1044 cm⁻¹ and 963 cm⁻¹, and hydroxyl peaks at 632 cm⁻¹. Powder X-ray diffraction (XRD) analysis showed prominent peaks at 2θ values of 25.9°, 32.2°, 39.8°, and 46.7°, corresponding to the crystalline planes of HAp. Field-emission scanning electron microscopy (FESEM) revealed spherical HAp particles with sizes ranging from 50 to 80 nm. Biocompatibility was assessed using human osteoblast-like MG-63 cells, showing a proliferation rate of 92 % compared to the control. Cytotoxicity tests indicated no significant adverse effects, supporting the potential use of this HAp in biomedical applications. Importantly, this method offers a sustainable solution for managing fish bone waste, contributing to pollution control by reducing environmental burdens associated with discarded bone wastes. Future research will focus on in vivo biocompatibility studies and exploring applications in pollution mitigation and tissue engineering. This study highlights the dual benefits of utilizing biowaste for valuable HAp production and addressing environmental pollution challenges, making it a promising approach for sustainable material synthesis and environmental management. The cost-effective and environmentally friendly process further underscores the feasibility of scaling up this method for industrial applications, providing a greener alternative to conventional HAp synthesis.

Synthesis and Characterization of Iron–Sillenite for Application as an XRD/MRI Dual-Contrast Agent

In the present work, iron–sillenite (Bi25FeO40) was synthesized using a simple solid-state reaction method and characterized. The effects of the synthesis conditions on the phase purity of Bi2O3/Fe3O4, morphological features, and possible application as an XRD/MRI dual-contrast agent were investigated. For the synthesis, the stoichiometric amounts of Bi2O3 and Fe3O4 were mixed and subsequently milled in a planetary ball mill for 10 min with a speed of 300 rpm. The milled mixture was calcined at various temperatures (550 °C, 700 °C, 750 °C, 800 °C, and 850 °C) for 1 h in air at a heating rate of 5 °C/min. For phase identification, powder X-ray diffraction (XRD) analysis was performed and infrared (FTIR) spectra were recorded. The surface morphology of synthesized samples was studied by field-emission scanning electron microscopy (FE-SEM). For the radiopacity measurements, iron–sillenite specimens were synthesized at different temperatures and mixed with different amounts of BaSO4 and Laponite solution. It was demonstrated that iron–sillenite Bi25FeO40 possessed sufficient radiopacity and could be a potential candidate to meet the requirements of its application as an XRD/MRI dual-contrast agent.

Quantifying pyrrhotite superstructures in copper-gold ore flotation through synchrotron X-ray diffraction analysis

Pyrrhotite, a significant sulfide mineral in base metal sulfide deposits, exists in various superstructures including magnetic (4C) and non-magnetic (5C and 6C) types. Identifying and quantifying pyrrhotite superstructures in an ore sample has been a challenge, hindering efforts to improve pyrrhotite rejection in copper–gold flotation. This study employed synchrotron X-ray powder diffraction (S-XRPD) analysis to quantify pyrrhotite superstructures in the concentrates obtained from flotation of a copper–gold ore after grinding with forged steel and 30% chromium grinding media. S-XRPD demonstrated a superior capability in detecting characteristic peaks of 4C, 5C and 6C pyrrhotite superstructures compared to conventional XRPD. Utilizing the Rietveld refinement method, the identified pyrrhotite superstructures were quantified. These findings were successfully validated through independent X-ray fluorescence analysis on elemental compositions. The quantification work demonstrated that 30% chromium grinding media enhanced the floatability of all pyrrhotite superstructures over forged steel grinding media and each pyrrhotite superstructure in the copper–gold ore resembled a copper sulfide mineral rather than pyrite in response to grinding media during flotation. This research highlights the potential of S-XRPD as an effective technique for identifying and quantifying pyrrhotite superstructures in ore samples and determining their flotation behaviors.

Larvicidal, bactericidal, antioxidant, hypoglycemic effects and anti-proliferative activity of phyto-synthesized Ag-ZnO nanocomposites using Eranthemum roseum (Vahl) R.Br. leaf extract against Aedes aegypti and Culex quinquefasciatus mosquito vectors

This research is conducted using zinc doped silver nanocomposite on Eranthemum roseum leaf extract. E. roseum has its own medicinal properties due its bioactive compounds. Silver and Zinc also has its own medicinal properties due to its microbial properties. Our work is aimed to combine nanoparticles with plant extract to explore the medicinal properties. The synthesized Ag-ZnO NCs is characterized using X-ray powder diffraction (XRD), Fourier-transform infrared spectroscopy (FTIR), Scanning electron microscopy with energy-dispersive X-ray spectroscopy (SEM-EDAX) and Transmission Electron Microscopy (TEM) analysis. The XRD analysis confirms the crystal nature of the Ag-ZnO NCs. The average shape of the nanocomposite was obtained using SEM as spherical, EDAX analysis confirming the presence of Ag, Zn and Oxygen and TEM conforms the oval shape of nanoparticles Antibacterial activity shows highest level of activity against K. pneumoniae and B. subtilis. DPPH Activity of Ag-ZnO NCs highest inhibition of 52.56 % while the ABTS analysis of Ag-ZnO NCs shows 54.28 %. Hypoglycemic activity α-amylase and α- glucosidase assay of Ag-ZnO NCs obtained good activity with maximum level of inhibition 63 % and 60 %. Anti-proliferative assay shows good activity against cancer causing cells in HepG2 human liver cancer line with 67.11 %. Larvicidal potential of Ag-ZnO NCs recorded good mortality rate against Aedes aegypti and Culex quinquefasciatus. This study confirms the maximum activity of Ag-ZnO NCs and acts as Larvicidal, Anti-proliferative, Antioxidant, Hypoglycemic agents.

Candesartan Cilexetil Formulations in Mesoporous Silica: Preparation, Enhanced Dissolution In Vitro, and Oral Bioavailability In Vivo

Candesartan cilexetil (CC) is one of well-tolerated antihypertensive drugs, while its poor solubility and low bioavailability limit its use. Herein, two mesoporous silica (Syloid XDP 3150 and Syloid AL-1 FP) and the corresponding amino-modified products (N-XDP 3150 and N-AL-1 FP) have been selected as the carriers of Candesartan cilexetil to prepare solid dispersion through solvent immersion, and characterized through using powder X-ray diffraction analysis, infrared spectroscopy, differential scanning calorimetry, scanning electron microscopy, and solid-state nuclear magnetic resonance spectroscopy, etc. The state of CC changed from crystalline to amorphous after loading onto the silica carriers, in which no interactions between CC and silica existed. Then, the dissolution behaviors in vitro were studied through using flow-through cell dissolution method. CC-XDP 3150 sample exhibited the most extensive dissolution, and the cumulative release of CC from it was 1.88-fold larger than that of CC. Moreover, the pharmacokinetic results in rats revealed that the relative bioavailability of CC-XDP 3150 and CC-N-XDP 3150 solid dispersions were estimated to be 326 % % and 238 % % in comparison with CC, respectively. Clearly, pore size, pore volume, and surface properties of silica carrier have remarkable effect on loading, dissolution and bioavailability of CC. In brief, this work will provide valuable information in construction of mesoporous silica-based delivery system toward poorly water-soluble drugs.

A comparative analysis of crustacean exoskeletons: structural, microstructural, morphological, and UV absorption studies

This study aims to investigate the structural, thermal, and spectral characteristics, along with the ultra-violet (UV) absorption of various marine benthos exoskeletons, such as various species of crabs (Portunus sanguinolentus, Portunus pelagicus, Charybdis feriata) and mantis shrimp (Oratosquilla oratoria). Their unique properties and ability to survive in harsh oceanic environments make them interesting research subjects. This research utilized powder x-ray diffraction (XRD) analysis to determine the crystal structure of the benthic varieties. The sample surface was analyzed using high-resolution micrographs obtained from field-emission scanning electron microscopy (FESEM), which identified the presence of chitin and calcite in the marine benthos. This was further confirmed by differential scanning calorimetry (DSC), and Fourier transform infrared spectroscopy (FTIR). The optical characteristics were investigated using UV-visible spectroscopy. The proximate analysis revealed high protein content in the mantis shrimp exoskeleton compared to other crab species, highlighting its excellent UV absorption characteristics. Overall, this research has the potential to broaden our understanding of marine organisms, which can have potential applications in biotechnology and materials science to develop nature-inspired innovative materials sustainably.

Exploring synthesis and annealing influence on WS2 (tungsten disulfide): Structural, morphological, optical, and magnetic profiles

The resurgence of interest in Transition Metal Dichalcogenides (TMDCs) stems from their remarkable magnetic and optical properties, reminiscent of graphene. TMDCs like MoS2, MoSe2, WS2, and WSe2 exhibit substantial bandgaps that shift from indirect to direct in single layers. This characteristic enables diverse applications such as solar cells, transistors, photodetectors, and electroluminescent devices, without the direct use of graphene. In this study, polycrystalline WS2 powder was synthesized via the solid-state reaction method. We systematically investigated the structural, morphological, optical, and magnetic properties concerning the synthesized WS2 and its variants annealed at different temperatures. Through X-ray powder diffraction (XRD) analysis, we confirmed the hexagonal structure of the as-synthesized compound, with a space group of P 63/mmc. Interestingly, no structural transitions were observed in the annealed samples. Morphological examination revealed a plate-like structure across all samples. The determination of the optical bandgap was facilitated by UV-DRS absorption spectrum analysis. Our findings showcased the ferromagnetic behavior of the synthesized WS2, corroborated by magnetic measurements and electron paramagnetic resonance (EPR) analysis. These insights contribute to a deeper understanding of TMDCs and pave the way for their tailored utilization in advanced technological applications.

Green synthesis of silver nanoparticles from Brassaiopsis hainla extract for the evaluation of antibacterial and anticorrosion properties

Plant-mediated synthesis of silver nanoparticles (AgNPs) is an eco-friendly and convenient alternative to conventional methods. Brassaiopsis hainla (B. hainla) leaf extract (BHE) was used in this study to reduce metal salts and cap and stabilize nanoparticles (NPs), which were characterized and tested for antibacterial and anti-corrosion properties. Stirring the B. hainla extract with AgNO3 led to a color change, indicating nanoparticle formation. The absorption peak at 428 nm in the UV–visible spectrum further validated its formation. The AgNPs were characterized using various techniques such as FTIR, UV–visible, PXRD, HRTEM, SEM, and EDX. Powder X-ray diffraction analysis confirmed its nanocrystalline nature, with an average crystallite size of 17.92 nm. The FTIR spectrum showed hydroxyl, amine, amide, and carbonyl groups as capping and reducing agents for the AgNPs. SEM analysis revealed poly-dispersed NPs of various sizes, while EDX showed an intense peak for Ag, and TEM images revealed mostly hexagonal and triangular NPs. Antibacterial activity was tested against three human pathogens: Staphylococcus aureus (S. aureus), Pseudomonas, and Klebsiella oxytoca (K. oxytoca). Significant antibacterial activity was observed specifically against K. oxytoca, with an 11 mm inhibition zone. Both plant extracts and AgNPs inhibited acid-induced corrosion, with the highest inhibition efficiencies of 81.69 % and 69.54 % at 1000 ppm, respectively. With rising concerns over bacterial resistance and metal corrosion, this study addresses global challenges related to new antimicrobial agents, which are crucial for combating antibiotic resistance and protecting metals in various industries.

The role of thickness on the structural and luminescence properties of Y2O3:Ho3+, Yb3+ upconversion films

The structural, surface, and upconversion (UC) luminescence properties of Y2O3:Ho3+,Yb3+ films grown by pulsed laser deposition, for different numbers of laser pulses, were studied. The crystallinity, surface, and UC luminescence properties of the thin films were found to be highly dependent on the number of laser pulses. The X-ray powder diffraction analysis revealed that Y2O3:Ho3+,Yb3+ films were formed in a cubic structure phase with an Ia 3¯\\documentclass[12pt]{minimal} \\usepackage{amsmath} \\usepackage{wasysym} \\usepackage{amsfonts} \\usepackage{amssymb} \\usepackage{amsbsy} \\usepackage{mathrsfs} \\usepackage{upgreek} \\setlength{\\oddsidemargin}{-69pt} \\begin{document}$$\\overline{3 }$$\\end{document} space group. The thicknesses of the films were estimated by using cross-sectional scanning electron microscopy, depth profiles using X-ray photoelectron spectroscopy (XPS), and the Swanepoel method. The high-resolution XPS was used to determine the chemical composition and oxidation states of the prepared films. The UC emissions were observed at 538, 550, 666, and 756 nm, assigned to the 5F4 → 5I8, 5S2 → 5I8, 5F5 → 5I8, and 5S2 → 5I7 transitions of the Ho3+ ions. The power dependence measurements confirmed the involvement of a two-photon process in the UC process. The color purity estimated from the Commission International de I’Eclairage coordinates confirmed strong green UC emission. The results suggested that the Y2O3:Ho3+,Yb3+ UC transparent films are good candidates for various applications, including solar cell applications.

A Congruent-Melt Infrared Nonlinear Optical Crystal Na4SrAs2S8.

A quaternary metal thioarsenate infrared (IR) nonlinear optical (NLO) compound Na4SrAs2S8 was successfully prepared by a high-temperature reaction method from stoichiometric agents. It crystallizes in the tetragonal P4n2 with the unit cell parameters a = 10.0393(3) Å, c = 6.9638(3) Å, and Z = 2, with the basic structural groups of isolated AsS4 tetrahedra. Compared with benchmark IR NLO crystal AgGaS2 (AGS), the title compound exhibits balanced optical properties of large band gap (3.05 eV vs. 2.60 eV) and considerable second harmonic generation response (0.95 × AGS). Moreover, the combined powder X-ray diffraction and differential scanning calorimetry analyses demonstrate that Na4SrAs2S8 is a congruent-melting compound with a low melting point of 668 °C, which is benefical for bulk single crystal growth. Experimental and theoretical calculation results indicate that Na4SrAs2S8 is a practically usable IR NLO crystal, also motivating the exploration of thioarsenates as high-performance IR NLO candidates.

FABRICATION AND CHARACTERIZATION OF ZnO:3,4-DIHYDRO-2H-NAPHTHO[2,3-b] [1,4] OXAZINE-5,10-DIONE THIN FILMS FOR SOLAR CELL APPLICATION

The fabricated films were characterized by SEM, EDX and Powder x-ray diffraction (XRD) analysis also their electrical activities were tested for the solarcell application. The films (1-5) are tested for their solar cell application. Film 4 shows minimum resistivity (ρ) value of 0.42X10-2Ωcm at 40% than that of the other films.

Chiral resolution of RS-ofloxacin through a novel diastereomeric cocrystal formation with L-glutamic acid by evaporative crystallization and quantification with capillary electrophoresis

Chiral drugs often exhibit significant differences in pharmacological activity between their enantiomers, highlighting the importance of effective chiral separation to enhance therapeutic efficacy and safety. Despite advances in this field, efficient methods for enantiomer separation remain a critical demand, especially for drugs like RS-Ofloxacin (RS-OFX), a chiral fluoroquinolone antibiotic. For RS-OFX, the S-enantiomer exhibits significantly higher potency—approximately 8–128 times greater—than the racemic mixture. This highlights the need to accurately separate the enantiomers. This study presents a new cocrystallization-based method for the precise and economical chiral separation of RS-OFX using amino acids by utilizing the formation of diastereomeric cocrystals. L-Glutamic acid (L-Glu) was identified as an appropriate coformer during the screening of potential coformers; consequently, diastereomeric cocrystals of R-OFX:L-Glu and S-OFX:L-Glu were successfully obtained. Melting point data, Fourier-Transform Infrared Spectroscopy (FTIR), and Powder X-Ray Diffraction (PXRD) analyses all confirmed the existence of a new solid state, revealing significant modifications in the crystal structure indicative of cocrystal formation. Capillary electrophoresis (CE) was employed to quickly identify the most suitable solvent mixture for the separation of the diastereomeric pair. The diastereomeric cocrystals exhibited distinct solubility profiles in various solvent mixtures, allowing effective chiral separation through evaporative crystallization in methanol:chloroform (50:50, v/v) mixture, yielding 61.82% enantiomeric excess (ee) of the more active S-OFX:L-Glu. The results of this study suggest that the chiral resolution of racemic APIs through diastereomeric cocrystal formation with amino acids has the potential for scalability and adaptability in other APIs. This approach has the potential to be a valuable tool for the pharmaceutical industry in improving the efficiency of producing enantiopure pharmaceuticals.

EVA implants for controlled drug delivery to the inner ear

This study evaluated the potential of poly(ethylene vinyl acetate) (EVA) copolymers as matrix formers in miniaturised implants, allowing to achieve controlled drug delivery into the inner ear. Due to the blood-cochlea barrier, it is impossible to reliably deliver a drug to this tiny and highly sensitive organ in clinical practice. To overcome this bottleneck, different EVA implants were prepared by hot melt extrusion, altering the vinyl acetate content and implant diameter. Dexamethasone was incorporated as a drug with anti-inflammatory and anti-fibrotic activity. Its release was measured into artificial perilymph, and the systems were thoroughly characterised before and after exposure to the medium by optical and scanning electron microscopy, SEM-EDX analysis, DSC, X-ray powder diffraction, X-ray microtomography and texture analysis. Notably, the resulting drug release rates were much higher than from silicone-based implants of similar size. Furthermore, varying the vinyl acetate content allowed for adjusting the desired release patterns effectively: With decreasing vinyl acetate content, the crystallinity of the copolymer increased, and the release rate decreased. Interestingly, the drug was homogeneously distributed as tiny crystals throughout the polymeric matrices. Upon contact with aqueous fluids, water penetrates the implants and dissolves the drug, which subsequently diffuses out of the device. Importantly, no noteworthy system swelling or shrinking was observed for up to 10 months upon exposure to the release medium, irrespective of the EVA grade. Also, the mechanical properties of the implants can be expected to allow for administration into the inner ear of a patient, being neither too flexible nor too rigid.

Nucleation, crystal growth, XRD, optical, electrical, PC, SEM, SHG and Z-scan analysis of LHPP for NLO and optical limiting application

High-quality organic L-histidinium 4-nitrophenolate 4-nitrophenol (LHPP) single crystals were grown using an aqueous solution. The crystals were grown using slow evaporation solution technique (SEST) at a temperature of 40°C using a constant temperature bath (CTB). Nucleation growth rates were monitored for various durations using an optical microscope. The crystalline perfection was confirmed through sharp, high-intensity diffraction peaks observed in the theoretical and experimental powder X-ray diffraction (PXRD) analysis, which also confirmed the monoclinic crystal structure with the noncentrosymmetric P21 space group. The crystallite size and strain were calculated using Williamson–Hall coefficient. Vibrational frequency assignments of LHPP were determined using FTIR spectroscopic analysis. Optical properties were studied using UV–Vis NIR spectroscopic studies, which showed that the crystals have very low absorption and high transmittance in the entire visible region. Additionally, the optical energy bandgap (Eg) was calculated and found to be 6.15[Formula: see text]eV. Luminescence properties were studied using fluorescence (FL) analysis. Dielectric investigations were subjected to varying frequencies to study the suitability of the crystal for transistor application. The positive photoconductive (PC) nature of the crystal was confirmed using photoconductivity studies to confirm suitability for photodetector devices that measure the intensity of light rays. Etching studies revealed the growth pattern and the formation of different kinds of etch pits. The surface morphology was studied using scanning electron microscopy (SEM) and electrochemical studies were also carried out. The relative second harmonic generation (SHG) efficiency of the material was also examined and found to be 1.34 times that of standard KDP. The optical limiting and higher-order nonlinear optical (NLO) properties of the grown crystals were studied by the [Formula: see text]-scan method using a Nd: YAG laser functioning at 532[Formula: see text]nm.

New Iron(III)-Containing Composite of Salinomycinic Acid with Antitumor Activity—Synthesis and Characterization

In this study we demonstrated for the first time synthetic procedures for composites of salinomycin (SalH) and two-line ferrihydrite. The products were characterized by various methods such as elemental analysis, attenuated total reflectance–Fourier-transform spectroscopy (ATR-FTIR), electron paramagnetic resonance spectroscopy (EPR), powder X-ray diffraction analysis (XRD), electrospray-ionization mass spectrometry (ESI-MS), thermogravimetric analysis with differential thermal analysis (DTA) and mass spectrometry (TG-DTA/MS). The EPR spectra of the isolated compounds consisted of signals associated with both isolated Fe3+ ions and magnetically coupled Fe3+ ions. Powder XRD analyses of the isolated products showed two intense and broad peaks at 9° and 15° 2Θ, corresponding to salinomycinic acid. Broad peaks with very low intensity around 35°, assigned to two-line ferrihydrite, were also registered. Based on the experimental results, we concluded that salinomycin sodium reacted with Fe(III) chloride to form composites consisting of two-line ferrihydrite and salinomycinic acid. One of the composites exerted pronounced antitumor activity in the sub-micromolar concentration range against human cervical cancer (HeLa), non-small-cell lung cancer (A549), colon cancer (SW480), and ovarian teratocarcinoma (CH1/PA1) cells.

Unveiling spectroscopic behaviour and molecular features (DFT studies) of Exemestane-maleic acid cocrystal as model multicomponent system

The present study aimed to investigate the Exemestane - maleic acid (Ex-Mal) cocrystal using Fourier-transform Raman (FT-Raman), Fourier-transform Infrared (FT-IR), Powder X-ray Diffraction (PXRD) and Differential Scanning Calorimeter (DSC) experimental techniques and quantum chemical calculations. Exemestane (Ex) is an irreversible aromatase inhibitor, clinically used for the treatment of postmenopausal women having primary or advanced breast cancer. Maleic acid (Mal), a dicarboxylic acid is found in many vegetables and fruits and is used as a food additive and sweetener. Solution crystallization of Ex and Mal was done in the generation of Ex-Mal cocrystal (1:1). PXRD and DSC analysis confirmed the successful generation of Ex-Mal Cocrystal. Intermolecular hydrogen bonding (O4-H12···O13 & C8-O3···H36) also suggested the formation of a multi-component system, Ex-Mal cocrystal (1:1), as the respective modes shifted in the vibrational (Raman & IR) spectra of cocrystal than the Ex. Further, the quantum theory of atoms in molecules (QTAIM) has been done to analyze the strength and nature of inter-/intra molecular hydrogen bonding. Natural bond orbital (NBO) analysis was performed to check the stabilization energy of the system. The frontier molecular orbital (FMO) analysis predicted that Ex-Mal cocrystal is more reactive and less stable than Ex. Molecular electrostatic potential (MEP) surface showed that electrophilic (C16-H36)/(O4-H12), and nucleophilic (C8=O3)/(C17=O13) reactive groups in Ex/Mal and Mal/Ex, respectively, neutralized after the formation of Ex-Mal cocrystal, confirming the presence of hydrogen bonding interactions (C16-H36∙∙∙O3=C8) and (C17=O13∙∙∙H12-O4). Molar Refractivity (MR) was calculated to check the drug-likeness behaviours of Ex-mal cocrystal. This study provided a comparison of experimental and theoretical results to understand the hydrogen bonding interactions and structural activity of the system.