scholarly journals Evaluation of Thermal-Induced Polymorphic Transformation on Desloratadine and Desloratadine-Benzoic Acid Salt

2020 ◽  
Vol 26 (4) ◽  
pp. 399-405
Author(s):  
Ahmad Ainurofiq ◽  
Rachmat Mauludin ◽  
Diky Mudhakir ◽  
Sundani Nurono Soewandhi
Keyword(s):  
Melting Point ◽  
Benzoic Acid ◽  
Polymorphic Transformation ◽  
Heating Process ◽  
X Ray Diffraction ◽  
Scanning Calorimetry ◽  
X Ray ◽  
Pharmaceutical Ingredients ◽  
Physicochemical Changes ◽  
Transformation Methods

Background: Active pharmaceutical ingredients face a challenge in manufacturing due to adverse physicomechanical properties. Desloratadine (DES) form I exhibits poor mechanical behavior through the formation of capping during the tableting process. Salt formation from DES and benzoic acid (BA) has been observed to resolve poor mechanical properties. However, the ability to withstand heat from the manufacturing process should be implemented in DES and DES-BA salt. The aim of this study was to determine the differences between thermal treatment results on DES and DES-BA salt and whether it causes them to undergo polymorphic transformation. Methods: Salt was crystallized between DES and BA using the solvent evaporation method. DES and DES-BA salt were heated at 110°C, 159°C (melting point of DES), 181°C (melting point of DES-BA), and 190°C. Following this, characterization was performed using differential scanning calorimetry (DSC), powder X-ray diffraction (PXRD), Fourier-transform infrared spectroscopy (FTIR), scanning electron microscopy (SEM), and solubility testing. Results: Polymorphic transformation caused by heat occurred in DES, but not in DES-BA salt. The transformation of DES was induced by the effect of heating, which changed polymorph I to a mixture of polymorph I and III at 110°C, to polymorph II at 159°C, and to a mixture of polymorph I, II, and III at 190°C. Under 190oC, DES-BA is still stable and did not undergo a polymorphic transformation. However, at 190oC, decomposition started to occur, which implied decreased solubility, which did not occur in DES. Conclusion: The heating process did not cause DES-BA salt to undergo a polymorphic transformation. However, it caused decomposition at 190oC. DES underwent a polymorphic transformation when exposed to the same condition without decomposition. This provided information to always pay attention to temperature during manufacturing processes that include DES or DES-BA salt to avoid physicochemical changes.

PHASE TRANSFORMATIONS DURING HEATING OF AMORPHOUS/NANOCRYSTALLINE Ni–Ti POWDERS

2010 ◽  
Vol 24 (09) ◽  
pp. 1137-1140 ◽  
Author(s):  
M. M. VERDIAN ◽  
M. SALEHI ◽  
K. RAEISSI
Keyword(s):  
Differential Scanning Calorimetry ◽  
Solid State ◽  
Phase Transformations ◽  
Low Energy ◽  
Heating Process ◽  
Study Phase ◽  
X Ray Diffraction ◽  
Scanning Calorimetry ◽  
X Ray ◽  
Niti Phase

Amorphous/nanocrystalline 50 Ni –50 Ti powders were synthesized from elemental Ti and Ni powders by solid state synthesis utilizing low energy mechanical alloying with times up to 100 h. The produced powders were investigated by X-ray diffraction and differential scanning calorimetry to study phase transformations that occurred during heating in the calorimeter. It was found that at the first stage of the heating process, a disordered NiTi phase was formed at temperature of about 400°C. Further investigations indicated that this phase transformed into the Ni 3 Ti and Ti 2 Ni intermetallic compounds after heating at a temperature of about 800°C.

scholarly journals The Usefulness of X-ray Diffraction and Thermal Analysis to Study Dietary Supplements Containing Iron

Molecules ◽  
2021 ◽  
Vol 27 (1) ◽  
pp. 197
Author(s):  
Izabela Jendrzejewska ◽  
Robert Musioł ◽  
Tomasz Goryczka ◽  
Ewa Pietrasik ◽  
Joanna Klimontko ◽  
...  
Keyword(s):  
Thermal Analysis ◽  
Melting Point ◽  
Dietary Supplements ◽  
Polymorphic Form ◽  
Food Supplements ◽  
X Ray Diffraction ◽  
Iron Compounds ◽  
Scanning Calorimetry ◽  
X Ray ◽  
Amorphous Compounds

X-ray powder diffraction (XRPD) and thermal analysis (differential scanning calorimetry/derivative of thermogravimetry (DSC/DTG)) are solid-state techniques that can be successfully used to identify and quantify various chemical compounds in polycrystalline mixtures, such as dietary supplements or drugs. In this work, 31 dietary supplements available on the Polish market that contain iron compounds, namely iron gluconate, fumarate, bisglycinate, citrate and pyrophosphate, were evaluated. The aim of the work was to identify iron compounds declared by the manufacturer as food supplements and to try to verify compliance with the manufacturer’s claims. Studies performed by X-ray and thermal analysis confirmed that crystalline iron compounds (iron (II) gluconate, iron (II) fumarate), declared by the manufacturers, were present in the investigated dietary supplements. Iron (II) bisglycinate proved to be semi-crystalline. However, depending on the composition of the formulation, it was possible to identify this compound in the tested supplements. For amorphous iron compounds (iron (III) citrate and iron (III) pyrophosphate), the diffraction pattern does not have characteristic diffraction lines. Food supplements containing crystalline iron compounds have a melting point close to the melting point of pure iron compounds. The presence of excipients was found to affect the shapes and positions of the endothermic peaks significantly. Widening of endothermic peaks and changes in their position were observed, as well as exothermic peaks indicating crystallization of amorphous compounds. Weight loss was determined for all dietary supplements tested. Analysis of the DTG curves showed that the thermal decomposition of most food supplements takes place in several steps. The results obtained by a combination of both simple, relatively fast and reliable XRPD and DSC/DTG methods are helpful in determining phase composition, pharmaceutical abnormalities or by detecting the presence of the correct polymorphic form.

scholarly journals Phase Transition and Melt-Recrystallization Behavior of Poly(Butylene Adipate) Investigated by Simultaneous Measurements of Wide-Angle X-Ray Diffraction (WAXD) and Differential Scanning Calorimetry (DSC)

Polymers ◽  
2020 ◽  
Vol 12 (1) ◽  
pp. 75
Author(s):  
Mengfan Wang ◽  
Weiyu Cao
Keyword(s):  
Phase Transition ◽  
Differential Scanning Calorimetry ◽  
Heating Process ◽  
Wide Angle ◽  
Melt Crystallization ◽  
X Ray Diffraction ◽  
Scanning Calorimetry ◽  
X Ray ◽  
Β Phase ◽  
Simultaneous Measurements

Simultaneous measurements of wide-angle X-ray diffraction (WAXD) and differential scanning calorimetry (DSC) were carried out to investigate the phase transition and melting behaviors of poly(butylene adipate) (PBA). Thermal expansion changes along the a and b axes of the β form unit cell are different from each other during the heating process. At the beginning of the β to αH (high-temperature α phase) phase transition, the β phase melts very fast, while the recrystallization of the αH phase is delayed and slowed. With the further increment of the temperature, the melting rate of the β phase slows down, while the recrystallization of the αH phase accelerates. The diffraction peak intensity ratios of the β(020):β(110) and αH(020):αH(110) diffraction peaks during the first heating process have similar value. However, the above value is different from the value of α(020):α(110) during the following melt-crystallization process. This difference comes from the different orientations of the crystal lattices of the α and αH(β) crystals to the substrate plane, which indicates that the αH phase inherits the orientation of the β phase during phase transition and the orientation of αH form crystals is different from the α form crystals that crystallized from the melt.

Solvates of the antifungal drug griseofulvin: structural, thermochemical and conformational analysis

2013 ◽  
Vol 70 (1) ◽  
pp. 54-62 ◽  
Author(s):  
Srinivasulu Aitipamula ◽  
Pui Shan Chow ◽  
Reginald B. H. Tan
Keyword(s):  
Melting Point ◽  
Solvent Free ◽  
Antifungal Drug ◽  
Free Form ◽  
Solution Stability ◽  
X Ray Diffraction ◽  
Scanning Calorimetry ◽  
X Ray ◽  
Solvent Molecules ◽  
Solid Form

Four solvates of an antifungal drug, griseofulvin (GF), were discovered. All the solvates were characterized by differential scanning calorimetry, thermogravimetric analysis, and their crystal structures were determined by single-crystal X-ray diffraction. The solvents that form the solvates are acetonitrile, nitromethane and nitroethane (2:1 and 1:1). It was found that all the solvates lose the solvent molecules from the crystal lattice between 343 and 383 K, and that the melting point of the desolvated materials matched the melting point of the solvent-free GF (493 K). The conformation of the GF molecule in solvent-free form was found to be significantly different from the conformations found in the solvates. Solution stability studies revealed that the GF–acetonitrile solvate transforms to GF and that GF–nitroethane (1:1) solvate transforms to GF–nitroethane (2:1) solvate. On the other hand, GF–nitromethane and GF–nitroethane (2:1) solvates were found to be stable in solution. Our results highlight the importance of the co-crystallization technique in the pharmaceutical drug development; it not only expands the solid form diversity but also creates new avenues for unraveling novel solvates.

scholarly journals Interconvertible Hydrochlorothiazide–Caffeine Multicomponent Pharmaceutical Materials: A Solvent Issue

Crystals ◽  
2020 ◽  
Vol 10 (12) ◽  
pp. 1088
Author(s):  
Cristóbal Verdugo-Escamilla ◽  
Carolina Alarcón-Payer ◽  
Antonio Frontera ◽  
Francisco Javier Acebedo-Martínez ◽  
Alicia Domínguez-Martín ◽  
...  
Keyword(s):  
Physicochemical Properties ◽  
Intermolecular Forces ◽  
Active Pharmaceutical Ingredients ◽  
X Ray Diffraction ◽  
Scanning Calorimetry ◽  
Great Stability ◽  
X Ray ◽  
Pharmaceutical Ingredients ◽  
Interesting Approach ◽  
Pharmaceutical Materials

The design of new multicomponent pharmaceutical materials that involve different active pharmaceutical ingredients (APIs), e.g., drug-drug cocrystals, is a novel and interesting approach to address new therapeutic challenges. In this work, the hydrochlorothiazide-caffeine (HCT–CAF) codrug and its methanol solvate have been synthesized by mechanochemical methods and thoroughly characterized in the solid state by powder and single crystal X-ray diffraction, respectively, as well as differential scanning calorimetry, thermogravimetric analyses and infrared spectroscopy. In addition, solubility and stability studies have also been performed looking for improved physicochemical properties of the codrug. Interestingly, the two reported structures show great similarity, which allows conversion between them. The desolvated HCT–CAF cocrystal shows great stability at 24 h and an enhancement of solubility with respect to the reference HCT API. Furthermore, the contribution of intermolecular forces on the improved physicochemical properties was evaluated by computational methods showing strong and diverse H-bond and π–π stacking interactions.

scholarly journals Melting Diagrams of Adefovir Dipivoxil and Dicarboxylic Acids: An Approach to Assess Cocrystal Compositions

Crystals ◽  
2019 ◽  
Vol 9 (2) ◽  
pp. 70 ◽  
Author(s):  
Hyunseon An ◽  
Insil Choi ◽  
Il Kim
Keyword(s):  
Solid State ◽  
Adefovir Dipivoxil ◽  
Sufficient Conditions ◽  
Dicarboxylic Acids ◽  
Current Approach ◽  
X Ray Diffraction ◽  
Scanning Calorimetry ◽  
X Ray ◽  
Pharmaceutical Ingredients ◽  
Solution Crystallization

Pharmaceutical cocrystallization is a useful method to regulate the physical properties of active pharmaceutical ingredients (APIs). Since the cocrystals may form in various API/coformer ratios, identification of the cocrystal composition is the critical first step of any further analysis. However, the composition identification is not always unambiguous if cocrystallization is performed in solid state with unsuccessful solution crystallization. Single melting point and some new X-ray diffraction peaks are necessary but not sufficient conditions. In the present study, the use of melting diagrams coupled with the X-ray diffraction data was tested to identify cocrystal compositions. Adefovir dipivoxil (AD) was used as a model API, and succinic acid (SUC), suberic acid (SUB), and glutaric acid (GLU) were coformers. Compositions of AD/SUC and AD/SUB had been previously identified as 2:1 and 1:1, but that of AD/GLU was not unambiguously identified because of the difficulty of solution crystallization. Melting diagrams were constructed with differential scanning calorimetry, and their interpretation was assisted by powder X-ray diffraction. The cocrystal formation was exhibited as new compositions with congruent melting in the phase diagrams. This method correctly indicated the previously known cocrystal compositions of AD/SUC and AD/SUB, and it successfully identified the AD/GLU cocrystal composition as 1:1. The current approach is a simple and useful method to assess the cocrystal compositions when the crystallization is only possible in solid state.

scholarly journals Multi-Component Crystals of 2,2′-Bipyridine with Aliphatic Dicarboxylic Acids: Melting Point-Structure Relations

Crystals ◽  
2021 ◽  
Vol 11 (10) ◽  
pp. 1151
Author(s):  
Vhukhudo Nethanani ◽  
Eustina Batisai
Keyword(s):  
Melting Point ◽  
Dicarboxylic Acids ◽  
Conformation Analysis ◽  
Solvent Evaporation Method ◽  
X Ray Diffraction ◽  
Melting Points ◽  
Scanning Calorimetry ◽  
X Ray ◽  
Aliphatic Dicarboxylic Acids ◽  
The Relationship

The aim of the study was to investigate the relationship between the melting point and the supramolecular structure of three multi-component crystals of aliphatic dicarboxylic acids with 2,2′-bipyridine and to investigate the conformations of 2,2′-bipyridine in published multi-component crystals. The crystals were prepared using the solvent evaporation method and were characterized using single-crystal X-ray diffraction (SCXRD), powder X-ray diffraction (PXRD), and differential scanning calorimetry (DSC). The crystal structures were further analyzed using CrystalExplorer, and the results were correlated with the melting points. The results of the conformation analysis of the reported multi-component crystals of 2,2′-bipyridine are also presented.

A new polymorphic form and polymorphic transformation of loratadine

RSC Advances ◽  
2016 ◽  
Vol 6 (88) ◽  
pp. 85063-85073 ◽  
Author(s):  
Ruimiao Chang ◽  
Qiang Fu ◽  
Pei Yu ◽  
Lu Wang ◽  
Yong Li ◽  
...  
Keyword(s):  
Electron Microscopy ◽  
Polymorphic Transformation ◽  
Polymorphic Form ◽  
Water Mixture ◽  
X Ray Diffraction ◽  
Scanning Calorimetry ◽  
Polarizing Microscopy ◽  
X Ray ◽  
New Form ◽  
Scanning Electron

In this work, a new form of loratadine (Form B) was prepared from a 20% methanol and 80% water mixture and characterized by polarizing microscopy, scanning electron microscopy, powder X-ray diffraction and differential scanning calorimetry.

scholarly journals Pengaruh Faktor Geografi Terhadap Karakteristik Bambu Petung

2019 ◽  
Vol 3 (1) ◽  
pp. 25-32
Author(s):  
Andromeda Dwi Laksono ◽  
Diah Tri Agustiningtyas
Keyword(s):  
Melting Point ◽  
Energy Dispersive Spectrometer ◽  
The Philippines ◽  
Phase Changes ◽  
Cubic Phase ◽  
X Ray Diffraction ◽  
Scanning Calorimetry ◽  
X Ray ◽  
Peak Value

In this study was about a comparison of geographic factors towards the characterization of petung bamboo in Indonesia and the Philippines. Bamboo is one of the plants that has advantages in the field of technical materials based on developments in composite materials and is found in various regions. In general, bamboo has lignin and cellulose, where the morphology and nature of both bamboos are not the same from different countries. Therefore,material testing was carried out on each Indonesian and Filipino petung bamboo using material characterization testing methods. The process of Differential Scanning Calorimetry (DSC) was carried out to measure calorimetry with the yield of melting point in Philippine petung bamboo at 341ºC which is lower than the melting point in Indonesian petung bamboo which is 354.34ºC. In this DSC test, quantitative and qualitative results were obtainedin the form of phase changes, melting, and transition temperatures that occurred. Then an Energy Dispersive Spectrometer (EDS) was analyzed and the carbon content of cellulose and lignin was higher in Indonesian petung bamboo, respectively 65.29 wt.% And 66.05 wt.%. The morphology of bamboo shows that the fibers and matrices present in Philippine petung bamboo are denser than those of Indonesian petung bamboo. The highest peak value based on X-Ray Diffraction (XRD) is found in Philippine petung bamboo at 2ș of 34.49 and cubic phase.

scholarly journals Study of possibility physical interactions antimalarial combination drugs

2020 ◽  
Author(s):  
Timbul Partogi H. Simorangkir
Keyword(s):  
Phase Diagram ◽  
Solid State ◽  
Melting Point ◽  
Crystal Habit ◽  
Supersaturated Solution ◽  
Physical Interaction ◽  
Contact Method ◽  
X Ray Diffraction ◽  
Scanning Calorimetry ◽  
X Ray

Identification of solid state to investigate the possibility of physical interaction between Antimalarial Artemisinin Combination Treatment base Artesunate (AS) and Amodiaquine (AQ) by hot contact method Kofler, cold contact method (crystallization reaction) and binary phase diagram confirmation had been carried out. The results of hot contact method Kofler shown the formation a new crystalline habit as a long and thin needle on the contact zone (mixing zone) between AS and AQ. A different melting point was seen in its single component. Cold contact methods between two of supersaturated solution of component AS and AQ in methanol solvent also indicated the growth of crystal habit as similar as hot contact method Kofler. Confirmation by biner phase diagram shown the specific diagram for cocrystalline phase. Solid state interaction between AS and AQ was analysed by powder X-ray diffraction, FTIR (Fourier Transformed Infra Red) spectrophotometric, microscopic SEM (Scanning Electron Microscopic) and thermal DTA (Differential Thermal Analysis), TG-DSC (Thermal Gravimetry- Differential Scanning Calorimetry). Microscopic analysis by SEM showed significantly the change of habit and morphology of crystal to long and thin needle shaped. The difference of powder X-ray diffraction (PXRD) interferences peaks were observed in addition to PXRD interference peaks of each component and its physical mixtures that proved formation of cocrystalline phase. DSC Thermogram indicated a new endothermic peak corresponding to melting point of a new cocrystalline phase at temperature 160,4°C.

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