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.

Mechanochemical synthesis insights and solid-state characterization of quininium aspirinate, a glass-forming drug–drug salt

2021 ◽  
Vol 77 (9) ◽  
Author(s):  
Nehemiah Harris ◽  
Jubilee Benedict ◽  
Diane A. Dickie ◽  
Silvina Pagola
Keyword(s):  
Crystal Structure ◽  
Differential Scanning Calorimetry ◽  
Ir Spectroscopy ◽  
Mechanochemical Synthesis ◽  
Mechanochemical Reaction ◽  
X Ray Diffraction ◽  
Scanning Calorimetry ◽  
X Ray ◽  
Ft Ir ◽  
Ft Ir Spectroscopy

Quinine (an antimalarial) and aspirin (a nonsteroidal anti-inflammatory drug) were combined into a new drug–drug salt, quininium aspirinate, C20H25N2O2 +·C9H7O4 −, by liquid-assisted grinding using stoichiometric amounts of the reactants in a 1:1 molar ratio, and water, EtOH, toluene, or heptane as additives. A tetrahydrofuran (THF) solution of the mechanochemical product prepared using EtOH as additive led to a single crystal of the same material obtained by mechanochemistry, which was used for crystal structure determination at 100 K. Powder X-ray diffraction ruled out crystallographic phase transitions in the 100–295 K interval. Neat mechanical treatment (in a mortar and pestle, or in a ball mill at 20 or 30 Hz milling frequencies) gave rise to an amorphous phase, as shown by powder X-ray diffraction; however, FT–IR spectroscopy unambiguously indicates that a mechanochemical reaction has occurred. Neat milling the reactants at 10 and 15 Hz led to incomplete reactions. Thermogravimetry and differential scanning calorimetry indicate that the amorphous and crystalline mechanochemical products form glasses/supercooled liquids before melting, and do not recrystallize upon cooling. However, the amorphous material obtained by neat grinding crystallizes upon storage into the salt reported. The mechanochemical synthesis, crystal structure analysis, Hirshfeld surfaces, powder X-ray diffraction, thermogravimetry, differential scanning calorimetry, FT–IR spectroscopy, and aqueous solubility of quininium aspirinate are herein reported.

scholarly journals Study on the Miscibility of Polypyrrole and Polyaniline Polymer Blends

2018 ◽  
Vol 2018 ◽  
pp. 1-5 ◽  
Author(s):  
Tekalign A. Tikish ◽  
Ashok Kumar ◽  
Jung Yong Kim
Keyword(s):  
Differential Scanning Calorimetry ◽  
Polymer Blends ◽  
Processing Method ◽  
Phase Behaviour ◽  
X Ray Diffraction ◽  
Scanning Calorimetry ◽  
X Ray ◽  
Amorphous Nature ◽  
Ft Ir

We report on the miscibility and phase behaviour of polypyrrole-polyaniline (PPy/PANI) as a function of blend composition. The PPy/PANI blends were prepared by solution processing method, using dimethyl sulfoxide (DMSO) solvent. Characterization of the polymer blends was carried out based on the data analysis from Fourier transform infrared spectroscopy (FT-IR), X-ray diffraction (XRD), and differential scanning calorimetry (DSC). The PPy/PANI system was successfully formed blends in DMSO solvent. The polymer blends showed almost amorphous nature in XRD spectra because of intermolecular interaction between PPy and PANI macromolecules, which was confirmed by FT-IR data. Specifically, the DSC result for the PPY : PANI = 50 : 50 wt.% blend showed only one glass transition temperature (Tg), which indicates that the two polymers are well miscible without undergoing any phase separation.

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.

Research on compatibility and surface of high impact bio-based polyamide

2021 ◽  
pp. 095400832110055
Author(s):  
Yang Wang ◽  
Yuhui Zhang ◽  
Yuhan Xu ◽  
Xiucai Liu ◽  
Weihong Guo
Keyword(s):  
Electron Microscopy ◽  
Mechanical Properties ◽  
Scanning Electron Microscopy ◽  
Differential Scanning Calorimetry ◽  
Crystallization Behavior ◽  
High Impact ◽  
X Ray Diffraction ◽  
Scanning Calorimetry ◽  
X Ray ◽  
Scanning Electron

The super-tough bio-based nylon was prepared by melt extrusion. In order to improve the compatibility between bio-based nylon and elastomer, the elastomer POE was grafted with maleic anhydride. Scanning Electron Microscopy (SEM) and Thermogravimetric Analysis (TGA) were used to study the compatibility and micro-distribution between super-tough bio-based nylon and toughened elastomers. The results of mechanical strength experiments show that the 20% content of POE-g-MAH has the best toughening effect. After toughening, the toughness of the super-tough nylon was significantly improved. The notched impact strength was 88 kJ/m2 increasing by 1700%, which was in line with the industrial super-tough nylon. X-ray Diffraction (XRD) and Differential Scanning Calorimetry (DSC) were used to study the crystallization behavior of bio-based PA56, and the effect of bio-based PA56 with high crystallinity on mechanical properties was analyzed from the microstructure.

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 Synthesis and mesomorphic properties of calamitic malonates and cyanoacetates tethered to 4-cyanobiphenyls

2012 ◽  
Vol 8 ◽  
pp. 371-378 ◽  
Author(s):  
Katharina C Kress ◽  
Martin Kaller ◽  
Kirill V Axenov ◽  
Stefan Tussetschläger ◽  
Sabine Laschat
Keyword(s):  
Differential Scanning Calorimetry ◽  
Ambient Temperature ◽  
Liquid Crystalline ◽  
X Ray Diffraction ◽  
Cyanoacetic Acid ◽  
Scanning Calorimetry ◽  
Isotropic Liquid ◽  
X Ray ◽  
Nematic Phases ◽  
Mesomorphic Properties

4-Cyano-1,1'-biphenyl derivatives bearing ω-hydroxyalkyl substituents were reacted with methyl 3-chloro-3-oxopropionate or cyanoacetic acid, giving liquid-crystalline linear malonates and cyanoacetates. These compounds formed monotropic nematic phases at 62 °C down to ambient temperature upon cooling from the isotropic liquid. The mesomorphic properties were investigated by differential scanning calorimetry, polarizing optical microscopy and X-ray diffraction (WAXS).

Inosose-Flüssigkristalle / Inosose Liquid Crystals

1990 ◽  
Vol 45 (7) ◽  
pp. 1084-1090 ◽  
Author(s):  
Klaus Praefcke ◽  
Bernd Kohne ◽  
Andreas Eckert ◽  
Joachim Hempel
Keyword(s):  
Differential Scanning Calorimetry ◽  
Liquid Crystal ◽  
High Temperature ◽  
Liquid Crystalline ◽  
Structural Features ◽  
Lyotropic Liquid Crystal ◽  
X Ray Diffraction ◽  
Scanning Calorimetry ◽  
X Ray ◽  
Alkyl Chains

Six S,S-dialkyl acetals 2a-f of inosose (1), tripodal in structure, have been synthesized, characterized and investigated by optical microscopy and differential scanning calorimetry (d.s.c.). The four S,S-acetals 2c-f with sufficiently long alkyl chains are thermotropic liquid crystalline; 2 e and 2 f are even dithermomesomorphic. Each of these four inosose derivatives 2c-f exhibits monotropically a most likely cubic mesophase (MI); in addition 2e and 2f show enantiotropically a hexagonal mesophase (Hx) with a non-covalent, supramolecular H-bridge architecture. Whereas the nature of the optically isotropic mesophase MI needs further clarification the stable high temperature mesophase Hx of 2 e and 2 f has been established by a miscibility test using a sugar S,S-dialkyl acetal also tripodal in structure and with a Hx phase proved by X-ray diffraction, but in contrast to 2 with an acyclic hydrophilic part. Similarities of structural features between the Hx-phases of 2e and 2f as well as of other thermotropic and lyotropic liquid crystal systems are discussed briefly.

scholarly journals Formation of Pharmaceutical Salts and Cocrystals via Vapour-Assisted Tumbling (VAT) – A Solvent Efficient Process with Potential Industrial Applications

2021 ◽  
Author(s):  
Alexander J. Stirk ◽  
Fabio E. S. Souza ◽  
Jenny Gerster ◽  
Fatemeh M. Mir ◽  
Avedis Karadeolian ◽  
...  
Keyword(s):  
Differential Scanning Calorimetry ◽  
Environmental Impact ◽  
Industrial Applications ◽  
X Ray Diffraction ◽  
Scanning Calorimetry ◽  
New Techniques ◽  
X Ray ◽  
Industry Standard ◽  
Pharmaceutical Salts ◽  
Solid Form

Crystallisations on both the academic and industrial scale often use large volumes of solvent. In order decrease the environmental impact of such processes, new techniques must be discovered that increase the efficiency of the solvents used. Introduced here is a process that combines repurposed industry standard hardware and aspects of mechanochemistry to produce a technique we call “Vapour Assisted Tumbling” (VAT). Pharmaceutical and well-known cocrystals and salts were formed by tumbling the coformers in an atmosphere of vaporised solvent, in this study, methanol (MeOH). This was done inside a custom built analogue of an industrial rotary cone dryer (RCD). It was found that a desired solid form could be obtained as monitored by powder X-ray diffraction and differential scanning calorimetry. By repurposing industrial RCDs, it is feasible that solid forms can be crystallised with both minimal and reusable/recyclable solvent – drastically lowering the environmental impact of such transformations.

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