scholarly journals Sulbactam pivoxil powder attributes and compatibility study with excipients

2021 ◽  
Vol 7 (1) ◽  
Author(s):  
Loreana C. Gallo ◽  
Noelia L. Gonzalez Vidal ◽  
Fabio F. Ferreira ◽  
María V. Ramírez-Rigo
Keyword(s):  
Thermal Analyses ◽  
Oral Route ◽  
Endothermic Peak ◽  
Compatibility Study ◽  
X Ray Diffraction ◽  
Scanning Calorimetry ◽  
Thermogravimetric Curve ◽  
Almost All ◽  
Potential Interactions ◽  
Lactamase Inhibitor

Abstract Background Sulbactam pivoxil is an irreversible β-lactamase inhibitor that can be used with β-lactam antibiotics to improve antibacterial therapy by the oral route. Relevant properties of this drug for pharmaceutical manufacturing are not available in the open literature. In this work, a solid-state characterization of sulbactam pivoxil at the molecular, particle, and bulk levels was performed. Results Particles exhibited a mean diameter of about 350 μm, irregular shape crystals, and good flow properties. This work presents for the first time the crystal structure of this β-lactamase inhibitor obtained by X-ray diffraction analysis. Fourier-transform infrared results showed the characteristic bands of aliphatic hydrocarbons and ester groups. The differential scanning calorimetry curve exhibited a sharp endothermic peak at 109 °C corresponding to sulbactam pivoxil melting. The thermogravimetric curve revealed a mass loss at 184 °C associated with a decomposition process. This powder showed a moisture content of 0.34% and a water activity of 0.463. Potential interactions between sulbactam pivoxil and common pharmaceutical excipients were evaluated by thermal analysis. The endothermic peak and the enthalpies of melting were preserved in almost all the analyzed mixtures. Conclusion The powder was constituted by micro-sized crystals of sulbactam pivoxil that had suitable physicochemical properties for processing in controlled humidity environments. Thermal analyses suggested that sulbactam pivoxil is compatible with most of the evaluated excipients. The information obtained in the present study is relevant for the development, manufacturing, and storage of formulations that include sulbactam pivoxil.

scholarly journals Curcumin and Quercetin-Loaded Nanoemulsions: Physicochemical Compatibility Study and Validation of a Simultaneous Quantification Method

Nanomaterials ◽  
2020 ◽  
Vol 10 (9) ◽  
pp. 1650
Author(s):  
Gustavo Richter Vaz ◽  
Adryana Clementino ◽  
Juliana Bidone ◽  
Marcos Antonio Villetti ◽  
Mariana Falkembach ◽  
...  
Keyword(s):  
Limit Of Detection ◽  
Biological Fluids ◽  
Thermal Analyses ◽  
Entrapment Efficiency ◽  
Compatibility Study ◽  
Scanning Calorimetry ◽  
Limit Of Quantification ◽  
X Ray ◽  
Simultaneous Quantification

Biphasic oil/water nanoemulsions have been proposed as delivery systems for the intranasal administration of curcumin (CUR) and quercetin (QU), due to their high drug entrapment efficiency, the possibility of simultaneous drug administration and protection of the encapsulated compounds from degradation. To better understand the physicochemical and biological performance of the selected formulation simultaneously co-encapsulating CUR and QU, a stability test of the compound mixture was firstly carried out using X-ray powder diffraction and thermal analyses, such as differential scanning calorimetry (DSC) and thermogravimetric analyses (TGA). The determination and quantification of the encapsulated active compounds were then carried out being an essential parameter for the development of innovative nanomedicines. Thus, a new HPLC–UV/Vis method for the simultaneous determination of CUR and QU in the nanoemulsions was developed and validated. The X-ray diffraction analyses demonstrated that no interaction between the mixture of active ingredients, if any, is strong enough to take place in the solid state. Moreover, the thermal analysis demonstrated that the CUR and QU are stable in the nanoemulsion production temperature range. The proposed analytical method for the simultaneous quantification of the two actives was selective and linear for both compounds in the range of 0.5–12.5 µg/mL (R2 > 0.9997), precise (RSD below 3%), robust and accurate (recovery 100 ± 5 %). The method was validated in accordance with ICH Q2 R1 “Validation of Analytical Procedures” and CDER-FDA “Validation of chromatographic methods” guideline. Furthermore, the low limit of detection (LOD 0.005 µg/mL for CUR and 0.14 µg/mL for QU) and the low limit of quantification (LOQ 0.017 µg/mL for CUR and 0.48 µg/mL for QU) of the method were suitable for the application to drug release and permeation studies planned for the development of the nanoemulsions. The method was then applied for the determination of nanoemulsions CUR and QU encapsulation efficiencies (> 99%), as well as for the stability studies of the two compounds in simulated biological fluids over time. The proposed method represents, to our knowledge, the only method for the simultaneous quantification of CUR and QU in nanoemulsions.

scholarly journals Reflectance Spectroscopy of Ammonium Salts: Implications for Planetary Surface Composition

Minerals ◽  
2020 ◽  
Vol 10 (10) ◽  
pp. 902
Author(s):  
Maximiliano Fastelli ◽  
Paola Comodi ◽  
Alessandro Maturilli ◽  
Azzurra Zucchini
Keyword(s):  
Surface Composition ◽  
Thermal Analyses ◽  
Laboratory Data ◽  
Structure Type ◽  
Reflectance Spectra ◽  
Careful Study ◽  
Scanning Calorimetry ◽  
Structural Environment ◽  
Almost All ◽  
Absorption Features

Recent discoveries have demonstrated that the surfaces of Mars, Ceres and other celestial bodies, as well as asteroids and comets, are characterized by the presence of ammonium-bearing minerals. A careful study of remote data compared with the analyses of more accurate laboratory data might allow a better remote characterization of planetary bodies. In this paper, the reflectance spectra of some ammoniated hydrous and anhydrous salts, namely sal-ammoniac NH4Cl, larderellite (NH4)B5O7(OH)2·H2O, mascagnite (NH4)SO4, struvite (NH4)MgPO4·6H2O and tschermigite (NH4)Al(SO4)2·12H2O, were collected at 293 and at 193 K. The aim is to detect how the NH4 vibrational features are affected by the chemical and structural environment. All samples were recovered after cooling cycles and were characterized by X-ray powder diffraction. Reflectance spectra of the studied minerals show absorption features around 1.3, 1.6, 2.06, 2.14, 3.23, 5.8 and 7.27 μm, related to the ammonium group. Between them, the 2ν3 at ~1.56 μm and the ν3 + ν4 at ~2.13 μm are the most affected modes by crystal structure type, with their position being strictly related to both anionic group and the strength of the hydrogen bonds. The reflectance spectra of water-rich samples [struvite (NH4)MgPO4·6(H2O) and tschermigite (NH4)Al(SO4)2·12(H2O)] show only H2O fundamental absorption features in the area from 2 to 2.8 μm and a band from hygroscopic water at 3 μm. Thermal analyses (TA), thermal gravimetry (TG) and differential scanning calorimetry (DSC) allowed to evaluate the dehydration temperatures and the occurring phase transitions and decompositions in the analyzed samples. In almost all samples, endothermic peaks at distinct temperatures were registered associated to loss of water molecules, differently linked to the structures. Moreover, an endothermic peak at 465 K in sal-ammoniac was associated to the phase transition from CsCl to NaCl structure type.

Synthetic norsethite, BaMg(CO3)2: revised crystal structure, thermal behaviour and displacive phase transition

2014 ◽  
Vol 78 (7) ◽  
pp. 1589-1611 ◽  
Author(s):  
H. Effenberger ◽  
T. Pippinger ◽  
E. Libowitzky ◽  
C. L. Lengauer ◽  
R. Miletich
Keyword(s):  
Crystal Structure ◽  
Oxygen Atom ◽  
Single Crystal ◽  
Thermal Analyses ◽  
X Ray Diffraction ◽  
Scanning Calorimetry ◽  
X Ray ◽  
Displacive Phase Transition ◽  
Changing Trend

AbstractThe crystal structure of synthetic BaMg(CO3)2 whose mineral name is norsethite was re-investigated by single-crystal X-ray diffraction. Complementary in situ high- and low-temperature studies by means of vibrational spectroscopy (Raman, IR), powder X-ray diffraction techniques and thermal analyses were performed. Diffraction images (298 K) revealed weak superstructure reflections caused by the displacement of the O atoms in the earlier considered Rm structure model (a = 5.0212(9), cnew = 2 cold = 33.581(6) Å , Rc, Z = 6, R1 = 0.011, sinθ/λ < 0.99 Å –1). Thermal analyses reveal decarbonatization in two decomposition steps above 750 K, and the heat-flow curves (difference scanning calorimetry) give clear evidence of a weak and reversible endothermal change at 343±1 K. This agrees with a discontinuity in the IR and single-crystal Raman spectra. The changing trend of the c/a ratio supports this discontinuity indicating a temperature-induced structural transition in the range between 343 and 373 K. As the change of the unit-cell volume is almost linear, the character of the transition is apparently second order and matches the mechanism of a subtle displacement of the oxygen atom position. The apparent instability of the Rc structure is also evidenced by the remarkably larger anisotropic displacement of the oxygen atom.

scholarly journals Synthesis, Structure and NH3 Sorption Properties of Mixed Mg1-xMnx(NH3)6Cl2 Ammines

Energies ◽  
2020 ◽  
Vol 13 (11) ◽  
pp. 2746 ◽  
Author(s):  
Perizat Berdiyeva ◽  
Anastasiia Karabanova ◽  
Jakob B. Grinderslev ◽  
Rune E. Johnsen ◽  
Didier Blanchard ◽  
...  
Keyword(s):  
Thermal Analyses ◽  
Activation Energies ◽  
Metal Halide ◽  
Sorption Properties ◽  
X Ray Diffraction ◽  
Scanning Calorimetry ◽  
X Ray ◽  
Mixed Metal ◽  
Temperature Range

This paper describes the synthesis, crystal structure, and NH3 sorption properties of Mg1-xMnx(NH3)6Cl2 (x = 0–1) mixed metal halide ammines, with reversible NH3 storage capacity in the temperature range 20–350 °C. The stoichiometry (x) dependent NH3 desorption temperatures were monitored using in situ synchrotron radiation powder X-ray diffraction, thermogravimetric analysis, and differential scanning calorimetry. The thermal analyses reveal that the NH3 release temperatures decrease in the mixed metal halide ammines in comparison to pure Mg(NH3)6Cl2, approaching the values of Mn(NH3)6Cl2. Desorption occurs in three steps of four, one and one NH3 moles, with the corresponding activation energies of 54.8 kJ⋅mol-1, 73.2 kJ⋅mol-1 and 91.0 kJ⋅mol-1 in Mg0.5Mn0.5(NH3)6Cl2, which is significantly lower than the NH3 release activation energies of Mg(NH3)6Cl2 (Ea = 60.8 kJ⋅mol-1, 74.8 kJ⋅mol-1 and 91.8 kJ⋅mol-1). This work shows that Mg1-xMnx(NH3)yCl2 (x = 0 to 1, y = 0 to 6) is stable within the investigated temperature range (20–350 °C) and also upon NH3 cycling.

Microstructures and Synthesis of Noble Metal-Based Bulk Metallic Glasses (Zr-Be-Ni-Ti)

2016 ◽  
Vol 17 ◽  
pp. 1-6
Author(s):  
M. Abo-Elsoud
Keyword(s):  
Metallic Glasses ◽  
Thermal Analyses ◽  
Bulk Metallic Glasses ◽  
High Energy ◽  
X Ray Diffraction ◽  
Scanning Calorimetry ◽  
Transmission Electron ◽  
Stage Crystallization ◽  
Energy Ball ◽  
Experimental Findings

High-energy ball-milling in hexane medium was employed to prepare Nobel Zr-based bulk metallic glasses (BMGs) alloy of three different nominal compositions Zr47Be23Ni15Ti15, Zr50Be20Ni15Ti15 and Zr52Be18Ni15Ti15, numbers indicate at.%). The glass forming ability was found to increase with decreasing Zr and increasing Be content, which can be ascribed to the enhanced atomic size mismatch of the constituents on Be addition. Amorphous Zr47Be23Ni15Ti15 powder undergoes two-stage crystallization with onset temperatures at 640 and 700 K and glass transition temperature Tg at 566 K. In contrast, the Zr50Be20Ni15Ti15 and Zr52Be18Ni15Ti15 samples remained crystalline to a certain extent even after prolonged milling and contained FCC Zr crystallites. Structural characterization was done by X-ray diffraction (XRD) and transmission electron microscopy (TEM). In addition, thermal analyses were performed by means of differential scanning calorimetry (DSC) thermogram to justify the experimental findings.

scholarly journals Different approaches to obtain functionalized alumina as additive in polymer electrolyte membranes

2021 ◽  
Author(s):  
Lucia Mazzapioda ◽  
Mirko Sgambetterra ◽  
Akiko Tsurumaki ◽  
Maria Assunta Navarra
Keyword(s):  
Fuel Cell ◽  
Aluminum Oxide ◽  
Thermal Analyses ◽  
Sol Gel ◽  
X Ray Diffraction ◽  
Scanning Calorimetry ◽  
Composite Electrolyte ◽  
Fuel Cell Performance ◽  
Operation Temperature ◽  
Electrolyte Membranes

AbstractA series of sulfated aluminum oxides (S-Al2O3), investigated as an electrolyte additive in Nafion membranes, was synthesized via three different methods: (i) sol–gel sulfation starting from an aluminum alkoxide precursor, (ii) room temperature sulfation of fumed aluminum oxide, and (iii) hydrothermal sulfation of fumed aluminum oxide. Through the characterization of the synthesized S-Al2O3 by means of X-ray diffraction (XRD), thermogravimetric analysis (TGA), and infrared (IR) spectroscopy, a higher sulfation rate was found to be achieved via a hydrothermal sulfation, and the coordination state of sulfate groups was identified as monodentate. By using this hydrothermally synthesized S-Al2O3 as additive, a composite Nafion-based membrane was realized and compared to plain Nafion, by means of thermal analyses and fuel cell tests. Although higher hydration degree was found for the undoped membrane by differential scanning calorimetry (DSC), improved retention of fuel cell performance upon the increase of operation temperature was observed by using the composite electrolyte, confirming the stabilizing effect of the acidic inorganic additive.

scholarly journals Curcumin and Quercetin Loaded Nanoemulsion: Physicochemical Compatibility Study and Validation of a Simultaneous Quantification Method

2020 ◽  
Author(s):  
Gustavo Vaz ◽  
Adryana Clementino ◽  
Juliana Bidone ◽  
Marcos Villetti ◽  
Mariana Falkembach ◽  
...  
Keyword(s):  
Biological Fluids ◽  
Thermal Analyses ◽  
Entrapment Efficiency ◽  
Compatibility Study ◽  
Stability Studies ◽  
Scanning Calorimetry ◽  
X Ray ◽  
Simultaneous Quantification ◽  
Biological Performance

Biphasic oily/water nanoemulsions have been proposed as delivery systems for the intranasal administration of curcumin (CUR) and quercetin (QU), due to their high drug entrapment efficiency, the possibility of simultaneous drug administration and protection of the encapsulated compounds from the degradation. To better understand the physicochemical and biological performance of the selected formulation simultaneously co-encapsulating CUR and QU, a stability test of the compounds mixture was firstly carried out using X-ray powder diffraction and thermal analyses, such as differential scanning calorimetry (DSC) and thermogravimetric analyses (TGA). The determination and quantification of the encapsulated active compounds was then required being an essential tool for the development of innovative nanomedicines. Thus, a new HPLC&ndash;UV/Vis method for the simultaneous determination of CUR and QU in the nanoemulsions and their evaluation in stability studies in simulated biological fluids was developed and validated. The X-ray diffraction analyses demonstrated that no interaction between the mixture of active ingredients, if any, is strong enough to take place in the solid state. Moreover, the thermal analysis demonstrated that the CUR and QU are stable in the nanoemulsion production temperature range. The proposed analytical method for the simultaneous quantification of the two actives was selective and linear for both compounds in the range of 0.5 &ndash; 12.5 &micro;g/mL (R2 &amp;gt; 0.9997), precise (RSD below 3%), robust and accurate (recovery 100 &plusmn; 5 %). The method was validated in accordance with ICH Q2 R1 &ldquo;Validation of Analytical Procedures&rdquo; and CDER-FDA 2validation of chromatographic methods&rdquo; guideline. Furthermore, the low detection (LOD &amp;lt; 0.005 &micro;g/mL for CUR and &amp;lt;0.14 &micro;g/mL for QU) and quantification limits (LOQ &amp;lt; 0.017 &micro;g/mL for CUR and &amp;lt; 0.48 &micro;g/mL for QU) of the method were suitable for the application to drug release and permeation studies planned for the development of the nanoemulsions. The method was then applied for the determination of nanoemulsions CUR and QU encapsulation efficiencies (&amp;gt; 99%), as well as for the stability studies of the two compounds in simulated biological fluids over time. The proposed method represents, to our knowledge, the only method for the simultaneous quantification of CUR, and QU in nanoemulsions.

PLGA+HA/βTCP scaffold incorporating simvastatin: a promising biomaterial for bone tissue engineering

2020 ◽  
Author(s):  
Mariane Beatriz Sordi ◽  
Ariadne Cristiane Cabral da Cruz ◽  
Águedo Aragones ◽  
Mabel Mariela Rodríguez Cordeiro ◽  
Ricardo de Souza Magini
Keyword(s):  
Tissue Engineering ◽  
Bone Tissue Engineering ◽  
Bone Tissue ◽  
Thermal Analyses ◽  
Chemical Properties ◽  
Biological Properties ◽  
Scanning Calorimetry ◽  
Evaporation Technique ◽  
Porosity Analysis ◽  
Biphasic Ceramic

The aim of this study was to synthesize, characterize, and evaluate degradation and biocompatibility of poly(lactic-co-glycolic acid) + hydroxyapatite / β-tricalcium phosphate (PLGA+HA/βTCP) scaffolds incorporating simvastatin (SIM) to verify if this biomaterial might be promising for bone tissue engineering. Samples were obtained by the solvent evaporation technique. Biphasic ceramic particles (70% HA, 30% βTCP) were added to PLGA in a ratio of 1:1. Samples with SIM received 1% (m:m) of this medication. Scaffolds were synthesized in a cylindric-shape and sterilized by ethylene oxide. For degradation analysis, samples were immersed in PBS at 37 °C under constant stirring for 7, 14, 21, and 28 days. Non-degraded samples were taken as reference. Mass variation, scanning electron microscopy, porosity analysis, Fourier transform infrared spectroscopy, differential scanning calorimetry, and thermogravimetry were performed to evaluate physico-chemical properties. Wettability and cytotoxicity tests were conducted to evaluate the biocompatibility. Microscopic images revealed the presence of macro, meso, and micropores in the polymer structure with HA/βTCP particles homogeneously dispersed. Chemical and thermal analyses presented very similar results for both PLGA+HA/βTCP and PLGA+HA/βTCP+SIM. The incorporation of simvastatin improved the hydrophilicity of scaffolds. Additionally, PLGA+HA/βTCP and PLGA+HA/βTCP+SIM scaffolds were biocompatible for osteoblasts and mesenchymal stem cells. In summary, PLGA+HA/βTCP scaffolds incorporating simvastatin presented adequate structural, chemical, thermal, and biological properties for bone tissue engineering.

Glibenclamide-Nicotinamide Cocrystals Synthesized by The Solvent Evaporation Method to Enhance Solubility and Dissolution Rate of Glibenclamide

2019 ◽  
Vol 9 (01) ◽  
pp. 21-26
Author(s):  
Arif Budiman ◽  
Ayu Apriliani ◽  
Tazyinul Qoriah ◽  
Sandra Megantara
Keyword(s):  
Solvent Evaporation ◽  
Physical Mixture ◽  
Dissolution Profile ◽  
Solvent Evaporation Method ◽  
X Ray Diffraction ◽  
Scanning Calorimetry ◽  
Evaporation Method ◽  
Dissolution Properties ◽  
Mixture Characterization

Purpose: To develop glibenclamide-nicotinamide cocrystals with the solvent evaporation method and evaluate their solubility and dissolution properties. Methods: Cocrystals of glibenclamide-nicotinamide (1:2) were prepared with the solvent evaporation method. The prediction of interactive cocrystals was observed using in silico method. The solubility and dissolution were performed as evaluation of cocrystals. The cocrystals also were characterized by differential scanning calorimetry (DSC), infrared spectrophotometry, and powder X-ray diffraction (PXRD). Result: The solubility and dissolution profile of glibenclamide-nicotinamide cocrystal (1:2) increased significantly compared to pure glibenclamide as well as its physical mixture. Characterization of cocrystal glibenclamide-nicotinamide (1:2) including infrared Fourier transform, DSC, and PXRD, indicated the formation of a new solid crystal phase differing from glibenclamide and nicotinamide. Conclusion: The confirmation of cocrystal glibenclamide-nicotinamide (1:2) indicated the formation of new solid crystalline phases that differ from pure glibenclamide and its physical mixture

Studies on the Preparation, Characterization and Solubility of -Cyclodextrin-Roxythromycin Inclusion Complexes

2009 ◽  
Vol 2 (2) ◽  
pp. 523-530
Author(s):  
D. Nagasamy Venkatesh ◽  
S. Karthick ◽  
M. Umesh ◽  
G. Vivek ◽  
R.M. Valliappan ◽  
...  
Keyword(s):  
Dissolution Rate ◽  
Inclusion Complexes ◽  
Phase Solubility ◽  
X Ray Diffraction ◽  
Scanning Calorimetry ◽  
X Ray ◽  
Ir Studies ◽  
Poorly Soluble ◽  
Poorly Soluble Drug

Roxythromycin/ β-cyclodextrin (Roxy/ β-CD) dispersions were prepared with a view to study the influence of β-CD on the solubility and dissolution rate of this poorly soluble drug. Phase-solubility profile indicated that the solubility of roxythromycin was significantly increased in the presence of β-cyclodextrin and was classified as AL-type, indicating the 1:1 stoichiometric inclusion complexes. Physical characterization of the prepared systems was carried out by differential scanning calorimetry (DSC), X-ray diffraction studies (XRD) and IR studies. Solid state characterization of the drug β-CD binary system using XRD, FTIR and DSC revealed distinct loss of drug crystallinity in the formulation, ostensibly accounting for enhancement of dissolution rate.

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