scholarly journals Synthesis, Characterization, and Intrinsic Dissolution Studies of Drug–Drug Eutectic Solid Forms of Metformin Hydrochloride and Thiazide Diuretics

Pharmaceutics ◽  
2021 ◽  
Vol 13 (11) ◽  
pp. 1926
Author(s):  
Guadalupe Coyote-Dotor ◽  
José C. Páez-Franco ◽  
Daniel Canseco-González ◽  
Alejandra Núñez-Pineda ◽  
Alejandro Dorazco-González ◽  
...  
Keyword(s):  
Solid State Nmr ◽  
Metformin Hydrochloride ◽  
Thiazide Diuretics ◽  
X Ray Diffraction ◽  
Spectroscopy Analysis ◽  
Intrinsic Dissolution ◽  
X Ray ◽  
Dissolution Properties ◽  
Binary Eutectic

The mechanochemical synthesis of drug–drug solid forms containing metformin hydrochloride (MET·HCl) and thiazide diuretics hydrochlorothiazide (HTZ) or chlorothiazide (CTZ) is reported. Characterization of these new systems indicates formation of binary eutectic conglomerates, i.e., drug–drug eutectic solids (DDESs). Further analysis by construction of binary diagrams (DSC screening) exhibited the characteristic V-shaped form indicating formation of DDESs in both cases. These new DDESs were further characterized by different techniques, including thermal analysis (DSC), solid state NMR spectroscopy (SSNMR), powder X-ray diffraction (PXRD) and scanning electron microscopy–energy dispersive X-ray spectroscopy analysis (SEM–EDS). In addition, intrinsic dissolution rate experiments and solubility assays were performed. In the case of MET·HCl-HTZ (χMET·HCl = 0.66), we observed a slight enhancement in the dissolution properties compared with pure HTZ (1.21-fold). The same analysis for the solid forms of MET·HCl-CTZ (χMET·HCl = 0.33 and 0.5) showed an enhancement in the dissolved amount of CTZ accompanied by a slight improvement in solubility. From these dissolution profiles and saturation solubility studies and by comparing the thermodynamic parameters (ΔHfus and ΔSfus) of the pure drugs with these new solid forms, it can be observed that there was a limited modification in these properties, not modifying the free energy of the solution (ΔG) and thus not allowing an improvement in the dissolution and solubility properties of these solid forms.

scholarly journals Synthesis of Metforminium Succinate by Melting. Crystal Structure, Thermal, Spectroscopic and Dissolution Properties

2017 ◽  
Vol 61 (3) ◽  
Author(s):  
Eduardo Plata-Vargas ◽  
Cinthia De la Cruz-Hernández ◽  
Alejandro Dorazco-González ◽  
Inés Fuentes-Noriega ◽  
David Morales-Morales ◽  
...  
Keyword(s):  
Sodium Succinate ◽  
Organic Salt ◽  
Metformin Hydrochloride ◽  
X Ray Diffraction ◽  
Melt Mixing ◽  
Intrinsic Dissolution ◽  
X Ray ◽  
Dissolution Properties ◽  
Ft Ir ◽  
Melting Crystal

The reaction by melt mixing at 220 °C of the antihyperglycemic drug metformin hydrochloride <strong>1</strong> with dehydrated sodium succinate yields efficiently the organic salt [MET]<sub>2</sub>[SUC] <strong>2</strong> (H-MET<sup>+</sup>= metforminium and SUC<sup>2-</sup> = succinate). Solid state CPMAS NMR <sup>13</sup>C spectroscopy experiments, powder X-ray diffraction and FT-IR results support the formation of the pharmaceutical salt <strong>2</strong> in good yields. Besides, the charged-assisted hydrogen bonding interactions of type N-H<sup>…-</sup>O(carboxylate) were thoroughly analyzed by single crystal X-Ray diffraction techniques. Thus, the pharmaceutical salt <strong>2</strong> possesses considerable thermal differences when compared to the pure starting reagents. In addition, intrinsic dissolution rate experiments in buffered aqueous solutions at pH= 6.8 showed a sustained-release behavior of the drug in <strong>2</strong> with a constant value of K<sub>int</sub> = 0.885 mg/min * cm<sup>2</sup>.

Characterization of some mesogenic alkyl 1-thioglycosides

2002 ◽  
Vol 80 (8) ◽  
pp. 1162-1165 ◽  
Author(s):  
B Henrissat ◽  
G K Hamer ◽  
M G Taylor ◽  
R H Marchessault
Keyword(s):  
Phase Transition ◽  
Liquid Crystal ◽  
Solid State ◽  
Solid State Nmr ◽  
Liquid Crystalline ◽  
Liquid Crystal Phase ◽  
X Ray Diffraction ◽  
X Ray ◽  
Liquid Crystalline Phases

A series of dodecyl 1-thio-β-D-glycosides has been synthesized and characterized (DSC, NMR, CP MAS, X-ray diffraction) as possible new marking materials with liquid-crystalline properties. These compounds undergo solid to liquid crystal phase transitions at various temperatures, which depend on the nature of the carbohydrate part of the structure. Their liquid-crystalline phases show extreme shear thinning behaviour.Key words: liquid crystal, powder X-ray diffraction, phase transition, thioglycoside, solid-state NMR, marking material

scholarly journals Characterization of a brazilian smectite by solid state NMR and X-ray diffraction techniques

1997 ◽  
Vol 8 (6) ◽  
pp. 581-586 ◽  
Author(s):  
Alcides Wagner Serpa Guarino ◽  
Rosane A. S. San Gil ◽  
Helena Polivanov ◽  
Sonia M.C. Menezes
Keyword(s):  
Solid State ◽  
Solid State Nmr ◽  
X Ray Diffraction ◽  
X Ray

Synthesis and Characterization of a New Copper(II) Complex with Nadolol, an Aminoalcoholic Beta-blocker. Crystal Structure of Na[Cu(nadololate)(CO3)] · H2O

2008 ◽  
Vol 63 (5) ◽  
pp. 543-547 ◽  
Author(s):  
Inés Viera ◽  
Laura Domínguez ◽  
Javier Ellena ◽  
María H. Torre
Keyword(s):  
Crystal Structure ◽  
Vibrational Spectroscopy ◽  
Copper Complex ◽  
Beta Blocker ◽  
Synthesis And Characterization ◽  
X Ray Diffraction ◽  
Spectroscopy Analysis ◽  
X Ray

This work reports the synthesis and characterization of a new copper complex with nadolol, a betablocker aminoalcohol. The stoichiometry found was Na[Cu(nadololate)(CO3)] · H2O. Electronic and vibrational spectroscopy analysis was performed, and the crystal structure of Na[Cu(nadololate)-(CO3)] · H2O was determined by X-ray diffraction.

Preparation and characterization of CuInS2 nanorods and nanotubes from an elemental solvothermal reaction

2001 ◽  
Vol 16 (10) ◽  
pp. 2805-2809 ◽  
Author(s):  
Yang Jiang ◽  
Yue Wu ◽  
Shengwen Yuan ◽  
Bo Xie ◽  
Shuyuan Zhang ◽  
...  
Keyword(s):  
Electron Microscopy ◽  
Transmission Electron Microscopy ◽  
Photoelectron Spectroscopy ◽  
Electron Transfer Reaction ◽  
Solvothermal Reaction ◽  
X Ray Diffraction ◽  
Spectroscopy Analysis ◽  
X Ray ◽  
Transmission Electron

A simple and convenient solvothermal reaction has been developed to produce CuInS2 nanorods and nanotubes from the elements in ethylenediamine at 280 °C. The products were characterized by x-ray diffraction, transmission electron microscopy, high-resolution transmission electron microscopy, scanning electron microscopy, and x-ray photoelectron spectroscopy. Analysis shows that the coordinating ability of ethylenediamine and the existence of liquid In may play important roles in the growth of one-dimension nanocrystallites and the electron-transfer reaction. In addition, spherical CuInS2 micrometer particles were obtained at 350 °C.

Darstellung und Charakterisierung des Silber(I,II,III)-oxidclathrates Ag7O8HCO3 / Synthesis and Characterization of the Silver(I,II,III) Oxide Clathrate Ag7O8HCO3

2000 ◽  
Vol 55 (9) ◽  
pp. 882-886 ◽  
Author(s):  
Martin Jansen ◽  
Sascha Vensky
Keyword(s):  
Electron Microscopy ◽  
Thermal Analysis ◽  
Scanning Electron Microscopy ◽  
Magnetic Susceptibility ◽  
Solid State Nmr ◽  
Synthesis And Characterization ◽  
X Ray Diffraction ◽  
X Ray ◽  
Scanning Electron

The silver(I,II,III) oxide clathrate Ag7O8HCO3 was synthesized by anodic oxidation of silver(I) in a suspension of Ag2CO3 in an aqueous AgF solution. The title compound was characterized by single crystal X-ray diffraction (cubic, Fm3̄m, a = 9.8085(3) Å, Z = 4), scanning electron microscopy, thermal analysis, IR spectroscopy, 1H-solid state-NMR and measurement of the magnetic susceptibility

Effect of texture on the intrinsic dissolution behaviour of acetylsalicylic acid and tolbutamide compacts

2007 ◽  
Vol 40 (5) ◽  
pp. 857-864 ◽  
Author(s):  
Mikko Tenho ◽  
Jaakko Aaltonen ◽  
Paula Heinänen ◽  
Leena Peltonen ◽  
Vesa-Pekka Lehto
Keyword(s):  
Acetylsalicylic Acid ◽  
Random Distribution ◽  
Preferred Orientation ◽  
X Ray Diffraction ◽  
Intrinsic Dissolution ◽  
X Ray ◽  
Dissolution Studies ◽  
Dissolution Properties ◽  
Dissolution Behaviour ◽  
Attachment Energy

Preferred orientation of crystallites,i.e.texture, is a common result when a sample with an irregular habit of particles is compacted to form a tablet. Since texturization alters the random distribution of the crystal planes on the surface of the compacted sample, the dissolution properties of highly texturized tablets could differ from the properties of a tablet with a less preferred orientation. Three batches from both acetylsalicylic acid and tolbutamide were recrystallized using different crystallization parameters to obtain powders with different texturization behaviour. Several X-ray diffraction procedures were used to characterize the texture and other crystallographic properties of the samples. The intrinsic dissolution profiles were measured using the channel flow technique. In addition, the attachment energy of the crystal planes lying on the surface of the compacts was calculated theoretically. The results indicate that the most texturized compacts had a clearly lower intrinsic dissolution rate than the compacts with a lower degree of preferred orientation. By combining the results of the texture measurements with the calculated attachment energy values, the surface energies of the samples could be estimated and the estimated energy values were in agreement with the results of the dissolution studies. Moreover, it was found that by using the results of the texture measurements, the habit of the sample particles can be successfully predicted.

scholarly journals NMR-Enhanced Crystallography Aids Open Metal-Organic Framework Discovery Using Solvent-Free Accelerated Aging

2019 ◽  
Author(s):  
Christopher A. O’Keefe ◽  
Cristina Mottillo ◽  
László Fábián ◽  
Tomislav Friscic ◽  
Robert W. Schurko
Keyword(s):  
Solid State Nmr ◽  
Metal Organic Framework ◽  
Accelerated Aging ◽  
Solvent Free ◽  
X Ray Diffraction ◽  
X Ray ◽  
Metal Organic ◽  
It Application ◽  
Organic Framework

NMR-enhanced crystallography enables the characterization of a novel cadmium-based, open metal-organic framework (MOF) from a solvent-free "accelerated aging" process. Whereas accelerated aging was devised as a clean, mild route for making MOFs, these results highlight how it application in materials discovery and characterization is aided by a combination of X-ray diffraction and solid-state NMR spectroscopy.<br>

scholarly journals Effect of Subsequent Aging in SiCP Reinforced AA2124 Aluminum Metal Matrix Composite

2009 ◽  
Vol 18 (5) ◽  
pp. 096369350901800 ◽  
Author(s):  
Yahya Bozkurt ◽  
Recep Artir ◽  
Hüseyin Uzun ◽  
Serdar Salman
Keyword(s):  
Metal Matrix ◽  
X Ray Diffraction ◽  
Spectroscopy Analysis ◽  
Subsequent Aging ◽  
X Ray ◽  
Aluminum Metal ◽  
Aluminum Metal Matrix Composite ◽  
Hardness Values ◽  
Scanning Electron

The present study is focused on the evaluation of the aging behaviour and microstructure characterization of AA2124/SiC/25p composite under the aging temperatures of 180, 185 and 190 °C for various dwelling time ranging from 0 up to 100 hours. The microstructure was characterized by means of scanning electron microscopy. The hardness, energy dispersive spectroscopy analysis and X-ray diffraction measurements were also performed to evaluate the characteristics of aged AA2124/SiC/25p composite. The results show that the hardness values of as-received composite were considerably improved up to two third by the subsequent aging. The hardness increasing was attributed to the presence of CuAl2, Al4SiC4 and precipitation phases in aged AA2124/SiC/25p composite.

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