scholarly journals Caffeine-Cyclodextrin Complexes as Solids: Synthesis, Biological and Physicochemical Characterization

2021 ◽  
Vol 22 (8) ◽  
pp. 4191
Author(s):  
Sebastian Szmeja ◽  
Tomasz Gubica ◽  
Andrzej Ostrowski ◽  
Aldona Zalewska ◽  
Łukasz Szeleszczuk ◽  
...  
Keyword(s):  
Physicochemical Characterization ◽  
The Body ◽  
High Toxicity ◽  
Solution Synthesis ◽  
X Ray Diffraction ◽  
Scanning Calorimetry ◽  
Caffeine Concentration ◽  
Ft Ir ◽  
Ir And Raman ◽  
Danio Rerio Embryos

Mechanochemical and in-solution synthesis of caffeine complexes with α-, β-, and γ-cyclodextrins was optimized. It was found that short-duration, low-energy cogrinding, and evaporation (instead of freeze-drying) are effective methods for the formation and isolation of these complexes. The products obtained, their pure components, and their mixtures were examined by powder X-ray diffraction (PXRD), differential scanning calorimetry (DSC), FT-IR and Raman spectroscopy. Moreover, molecular modeling provided an improved understanding of the association process between the guest and host molecules in these complexes. The complexes were found to exhibit high toxicity in zebrafish (Danio rerio) embryos, in contrast to pure caffeine and cyclodextrins at the same molar concentrations. HPLC measurements of the caffeine levels in zebrafish embryos showed that the observed cytotoxicity is not caused by an increased caffeine concentration in the body of the organism, as the concentrations are similar regardless of the administered caffeine form. Therefore, the observed high toxicity could be the result of the synergistic effect of caffeine and cyclodextrins.

scholarly journals Mechanochemical Synthesis and Physicochemical Characterization of Previously Unreported Praziquantel Solvates with 2-Pyrrolidone and Acetic Acid

Pharmaceutics ◽  
2021 ◽  
Vol 13 (10) ◽  
pp. 1606
Author(s):  
Debora Zanolla ◽  
Lara Gigli ◽  
Dritan Hasa ◽  
Michele R. Chierotti ◽  
Mihails Arhangelskis ◽  
...  
Keyword(s):  
Acetic Acid ◽  
Water Solubility ◽  
Physicochemical Characterization ◽  
X Ray Diffraction ◽  
Scanning Calorimetry ◽  
Pxrd Pattern ◽  
Intrinsic Dissolution ◽  
Ft Ir ◽  
Biopharmaceutical Properties

Two new solvates of the widely used anthelminthic Praziquantel (PZQ) were obtained through mechanochemical screening with different liquid additives. Specifically, 2-pyrrolidone and acetic acid gave solvates with 1:1 stoichiometry (PZQ-AA and PZQ-2P, respectively). A wide-ranging characterization of the new solid forms was carried out by means of powder X-ray diffraction, differential scanning calorimetry, FT-IR, solid-state NMR and biopharmaceutical analyses (solubility and intrinsic dissolution studies). Besides, the crystal structures of the two new solvates were solved from their Synchrotron-PXRD pattern: the solvates are isostructural, with equivalent triclinic packing. In both structures acetic acid and 2-pyrrolidone showed a strong interaction with the PZQ molecule via hydrogen bond. Even though previous studies have shown that PZQ is conformationally flexible, the same syn conformation as the PZQ Form A of the C=O groups of the piperazinone-cyclohexylcarbonyl segment is involved in these two new solid forms. In terms of biopharmaceutical properties, PZQ-AA and PZQ-2P exhibited water solubility and intrinsic dissolution rate much greater than those of anhydrous Form A.

Liquid crystalline polyureas with oligo(ethylene glycol) sequences

e-Polymers ◽  
2010 ◽  
Vol 10 (1) ◽  
Author(s):  
Shahram Mehdipour-Ataei ◽  
Leila Akbarian-Feizi
Keyword(s):  
Liquid Crystalline ◽  
Spectroscopic Method ◽  
Polymerization Reaction ◽  
X Ray Diffraction ◽  
Subsequent Reaction ◽  
Scanning Calorimetry ◽  
Polar Solvents ◽  
X Ray ◽  
H Nmr ◽  
Ft Ir

AbstractA diamine monomer containing ester, amide and ether functional groups was prepared and its polymerization reaction with different diisocyanates to give main chain poly(ester amide ether urea)s was investigated. The monomer was synthesized via reaction of terephthaloyl chloride with 4-hydroxybenzoic acid and subsequent reaction of the resulted diacid with 1,8-diamino-3,6-dioxaoctane. The polymers were characterized by FT-IR and 1H-NMR spectroscopic method and elemental analysis. The resulting polymers exhibited excellent solubility in polar solvents. Crystallinity of the resulted polymers was evaluated by wide-angle X-ray diffraction (WXRD) method, and they exhibited semi-crystalline patterns. The glass transition temperatures (Tg) of the polymers determined by differential scanning calorimetry (DSC) and dynamic mechanical thermal analysis (DMTA) were in the range of 88-112 °C. The temperatures for 10% weight loss (T10) from their thermogravimetric analysis (TGA) curves were found to be in the range of 297-312 °C in air. Also the prepared polyureas showed liquid crystalline character.

scholarly journals Novel solid forms of the analgesic drug ethenzamide

2014 ◽  
Vol 70 (a1) ◽  
pp. C995-C995
Author(s):  
Duane Choquesillo-Lazarte ◽  
Cristóbal Verdugo-Escamilla ◽  
Juan Manuel García-Ruiz
Keyword(s):  
Polycrystalline Material ◽  
X Ray Diffraction ◽  
Analgesic Drug ◽  
X Ray ◽  
Solution Methods ◽  
Additional Stability ◽  
Ft Ir ◽  
Model Drug ◽  
Solid Form ◽  
Ir And Raman

The interest in multicomponent solid forms has increased in the last years within the pharmaceutical industry and also the solid-state community due to the possibility of obtaining materials with new properties [1]. Crystallization strategies, supported by solvent- and solid-based techniques, have also received attention in the search and development of methodologies for the screening of multicomponent crystals. In this work, ethenzamide, an anti-inflammatory and analgesic drug, was selected as a model drug to develop cocrystals on the basis of the synthon types using a series of phenolic coformers. Ethenzamide cocrystals and cocrystal solvates have been reported recently [2,3]. Liquid Assisted Grinding (LAG) and solution methods were used as synthetic tools. Attempts to produce cocrystals by LAG and Reaction Crystallization led to the formation of polycrystalline material. The solids obtained were then characterized by powder X-ray diffraction (PXRD), FT-IR and Raman spectroscopy. Recrystallization by slow solvent evaporation was carried out when the above-referred techniques strongly suggest the formation of a new solid form. The structure of five new multicomponent solids has been determined by single crystal X-ray diffraction. Additional stability studies have been performed at controlled relative humidity conditions and followed by PXRD.

Synthesis and Properties of Thermotropic Liquid Crystalline Polyesters with Flexible Polymethylene Spacer

2010 ◽  
Vol 428-429 ◽  
pp. 126-131
Author(s):  
Wei Zhong Lu ◽  
Chun Wei ◽  
Qui Shan Gao
Keyword(s):  
Optical Microscopy ◽  
Liquid Crystalline ◽  
X Ray Diffraction ◽  
Scanning Calorimetry ◽  
X Ray ◽  
Structure Morphology ◽  
Temperature Ranges ◽  
Ft Ir ◽  
Diffraction Peaks ◽  
Ubbelohde Viscometer

Polymethylene bis(p-hydroxybenzoates) were prepared from methyl p-hydroxybenzoate and different diols by melted transesterification reaction. Three liquid crystalline polyesters were synthesized from terephthaloyl dichloride and polymethylene bis(p-hydroxybenzoates). Its structure, morphology and properties were characterized by Ubbelohde viscometer, Fourier transform infrared spectroscopy (FT-IR), Differential scanning calorimetry (DSC), polarized optical microscopy (POM) with a hot stage, and wide-angle X-ray diffraction (WAXD). Results indicated that the intrinsic viscosities were between 0.088 and 0.210 dL/g. Optical microscopy showed that the TLCP has a highly threaded liquid crystalline texture and a high birefringent schlieren texture character of nematic phase and has wider mesophase temperature ranges for all polyesters. DSC analysis were found that the melting point (Tm), isotropic temperature (Ti) of TLCPs decreased and the temperature range of the liquid crystalline phase became wider with increased number of methylene spacers in the polyester. The WAXD results showed that TLCPs owned two strong diffraction peaks at 2θ near 19° and 23°.

scholarly journals THE PHYSICOCHEMICAL CHARACTERISTICS OF RECYCLED-PLASTIC PELLETS OBTAINED FROM DISPOSABLE FACE MASK WASTES

2021 ◽  
Vol 23 (1) ◽  
pp. 16
Author(s):  
Vienna Saraswaty ◽  
Rossy Choerun Nissa ◽  
Bonita Firdiana ◽  
Akbar Hanif Dawam Abdullah
Keyword(s):  
Tensile Strength ◽  
Physicochemical Characterization ◽  
Face Mask ◽  
Physicochemical Characteristics ◽  
Scanning Calorimetry ◽  
Elongation At Break ◽  
Ft Ir ◽  
The Government ◽  
Plastic Pellets

THE PHYSICOCHEMICAL CHARACTERISTICS OF RECYCLED-PLASTIC PELLETS OBTAINED FROM DISPOSABLE FACE MASK WASTES. The government policy to wear a face mask during the COVID-19 pandemic has increased disposable face mask wastes. Thus, to reduce such wastes, it is necessary to evaluate the physicochemical characteristics of disposable face masks wastes before the recycling process and the recycled products. In this study, physicochemical characterization of the 3-ply disposable face masks and the recycled plastic pellets after disinfection using 0.5% v/v sodium hypochlorite were evaluated. A set of parameters including the characterization of surface morphology by a scanning electron microscope (SEM), functional groups properties by a fourier transform infra-red spectroscopy (FT-IR), thermal behavior by a differential scanning calorimetry (DSC), tensile strength and elongation at break were evaluated. The surface morphological of each layer 3-ply disposable face mask showed that the layers were composed of non-woven fibers. The FT-IR evaluation revealed that 3-ply disposable face mask was made from a polypropylene. At the same time, the DSC analysis found that the polypropylene was in the form of homopolymer. The SEM analysis showed that the recycled plastic pellets showed a rough and uneven surface. The FT-IR, tensile strength and elongation at break of the recycled plastic pellets showed similarity with a virgin PP type CP442XP and a recycled PP from secondary recycling PP (COPLAST COMPANY). In summary, recycling 3-ply disposable face mask wastes to become plastic pellets is recommended for handling disposable face mask wastes problem.

scholarly journals Optical, Structural and Electrical Properties of Electrochemical Synthesis of Thin Film of Polyaniline

2018 ◽  
Vol 15 (1) ◽  
pp. 73-80 ◽  
Author(s):  
Baghdad Science Journal
Keyword(s):  
X Ray Diffraction ◽  
X Ray ◽  
Force Microscopy ◽  
Morphological Studies ◽  
Atomic Force ◽  
Vis Spectroscopy ◽  
Structural And Electrical Properties ◽  
A Cell ◽  
Ft Ir ◽  
Ir And Raman

Polyaniline membranes of aniline were produced using an electrochemical method in a cell consisting of two poles. The effect of the vaccination was observed on the color of membranes of polyaniline, where analysis as of blue to olive green paints. The sanction of PANI was done by FT-IR and Raman techniques. The crystallinity of the models was studied by X-ray diffraction technique. The different electronic transitions of the PANI were determined by UV-VIS spectroscopy. The electrical conductivity of the manufactured samples was measured by using the four-probe technique at room temperature. Morphological studies have been determined by Atomic force microscopy (AFM). The structural studies have been measured by (SEM).

scholarly journals Sonochemical-assisted magnesium borate synthesis from different boron sources

2017 ◽  
Vol 19 (1) ◽  
pp. 81-88 ◽  
Author(s):  
Meral Yildirim ◽  
Azmi Seyhun Kipcak ◽  
Emek Moroydor Derun
Keyword(s):  
High Efficiency ◽  
Synthesis Method ◽  
Spectroscopic Studies ◽  
X Ray Diffraction ◽  
Magnesium Borate ◽  
Ir And Raman Spectroscopies ◽  
Ft Ir ◽  
Surface Morphologies ◽  
Ir And Raman ◽  
Good Agreement

Abstract In this study, sonochemical-assisted magnesium borate synthesis is studied from different boron sources. Various reaction parameters are successfully applied by a simple and green method. X-ray diffraction (XRD), Fourier transform infrared (FT-IR) and Raman spectroscopies are used to characterize the synthesized magnesium borates on the other hand surface morphologies are investigated by using scanning electron microscope (SEM). The XRD analyses showed that the products were admontite [MgO(B2O3)3 · 7(H2O)] with JCPDS (Joint Committee on Powder Diffraction Standards) no. of 01-076-0540 and mcallisterite [Mg2(B6O7(OH)6)2 · 9(H2O)] with JCPDS no. of 01-070-1902. The results that found in the spectroscopic studies were in a good agreement with characteristic magnesium borate bands in both regions of infra-red and visible. According to SEM results, obtained borates were in micro and sub-micro scales. By the use of ultrasonication, reaction yields were found between 84.2 and 97.9%. As a result, it is concluded that the sonochemical approach is a practicable synthesis method to get high efficiency and high crystallinity in the synthesis magnesium borate compounds.

Compatibility between Magnesium Stearate and Pharmaceutical Acidic Active Compounds/Excipients with DSC

2020 ◽  
Vol 856 ◽  
pp. 190-197
Author(s):  
Pornsit Chaiya ◽  
Thawatchai Phaechamud
Keyword(s):  
Differential Scanning Calorimetry ◽  
Magnesium Stearate ◽  
X Ray Diffraction ◽  
Salt Form ◽  
Scanning Calorimetry ◽  
Powder Mixtures ◽  
X Ray ◽  
Pharmaceutical Excipients ◽  
Drug Compounds ◽  
Ft Ir

Compatibility investigation was performed between magnesium stearate and acidic drug compounds (ibuprofen, indomethacin and valproic acid) and acidic pharmaceutical excipients (lactic acid and citric acid) using differential scanning calorimetry (DSC). DSC study indicated the possible incompatibility for the mixture between magnesium stearate and any compounds. Alteration in DSC thermogram was found in all mixtures. The eutectic phenomenon was found in the powder mixture of magnesium stearate and ibuprofen. In addition, the presence of melting endothermic peak of stearic acid in other powder mixtures except the mixture of magnesium stearate and indomethacin indicating breakage of salt form of magnesium stearate. This alteration could relate to the influence on physicochemical properties of drug compounds and pharmaceutical excipients which powder x-ray diffraction (PXRD) and Fourier Transform Infrared Spectroscopy (FT-IR) should be further analyzed to confirm the interactions between compounds.

Stress-Induced Crystal-to-Crystal Transformations in High-Density Polyethylene-Layered Silicate Nanocomposites: A Spectroscopic Study

2005 ◽  
Vol 59 (9) ◽  
pp. 1148-1154 ◽  
Author(s):  
Spiros Tzavalas ◽  
Vasilis G. Gregoriou
Keyword(s):  
High Density Polyethylene ◽  
Mechanical Strain ◽  
Layered Silicate ◽  
High Density ◽  
X Ray Diffraction ◽  
Scanning Calorimetry ◽  
Polyethylene Matrix ◽  
Dsc Measurements ◽  
Infrared Measurements ◽  
Ft Ir

High-density polyethylene (HDPE)–clay nanocomposites have been prepared using the melt intercalation technique. Organically modified montmorillonite at various loadings (0.5–7%) was used as a nanoadditive. Fourier transform infrared spectroscopy (FT-IR) was utilized for the first time to monitor the stress-induced crystal-to-crystal transformations of the polyethylene matrix with respect to the clay loading as well as to the degree of mechanical strain. In addition, polarized infrared measurements revealed information on both the orientation and the stress-induced distortion of the crystals. It was concluded that the crystal-to-crystal transformations are hindered by the presence of the clay, which also prevented the crystals from orienting even at low clay loadings (1%). Finally, X-ray diffraction (XRD) and differential scanning calorimetry (DSC) measurements confirmed the presence of the stress-induced crystalline structures in agreement with the infrared measurements.

scholarly journals Preparation and Properties of Ginger Essential Oil β-Cyclodextrin/Chitosan Inclusion Complexes

Coatings ◽  
2018 ◽  
Vol 8 (9) ◽  
pp. 305 ◽  
Author(s):  
Yan Zhang ◽  
Hui Zhang ◽  
Fang Wang ◽  
Li-Xia Wang
Keyword(s):  
Particle Size ◽  
Essential Oil ◽  
Spray Drying ◽  
Small Particle Size ◽  
X Ray Diffraction ◽  
Scanning Calorimetry ◽  
X Ray ◽  
Ft Ir ◽  
Thermal Stability Of ◽  
Scanning Electron

The ginger essential oil/β-cyclodextrin (GEO/β-CD) composite, ginger essential oil/β-cyclodextrin/chitosan (GEO/β-CD/CTS) particles and ginger essential oil/β-cyclodextrin/chitosan (GEO/β-CD/CTS) microsphere were prepared with the methods of inclusion, ionic gelation and spray drying. Their properties were studied by using scanning electron microscopy (SEM), differential scanning calorimetry (DSC), thermo-gravimetry analysis (TGA), Fourier transform infrared spectroscopy (FT-IR) and X-ray diffraction (XRD). The results showed that the particle size of GEO/β-CD composite was smaller than that of β-CD and GEO/β-CD/CTS particles were loose and porous, while the microsphere obtained by spray drying had certain cohesiveness and small particle size. Besides, results also indicated that β-CD/CTS could modify properties and improve the thermal stability of GEO, which would improve its application value in food and medical industries.

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