scholarly journals Pharmaceutical Hydrates Analysis—Overview of Methods and Recent Advances

Pharmaceutics ◽  
2020 ◽  
Vol 12 (10) ◽  
pp. 959
Author(s):  
Ewa Jurczak ◽  
Anna Helena Mazurek ◽  
Łukasz Szeleszczuk ◽  
Dariusz Maciej Pisklak ◽  
Monika Zielińska-Pisklak
Keyword(s):  
Resonance Spectroscopy ◽  
X Ray Diffraction ◽  
Hydration Kinetics ◽  
Scanning Calorimetry ◽  
X Ray ◽  
Degree Of Hydration ◽  
Pharmaceutical Ingredients ◽  
Fourier Transformed Infrared Spectroscopy ◽  
Ft Ir ◽  
Analytical Approaches

This review discusses a set of instrumental and computational methods that are used to characterize hydrated forms of APIs (active pharmaceutical ingredients). The focus has been put on highlighting advantages as well as on presenting some limitations of the selected analytical approaches. This has been performed in order to facilitate the choice of an appropriate method depending on the type of the structural feature that is to be analyzed, that is, degree of hydration, crystal structure and dynamics, and (de)hydration kinetics. The presented techniques include X-ray diffraction (single crystal X-ray diffraction (SCXRD), powder X-ray diffraction (PXRD)), spectroscopic (solid state nuclear magnetic resonance spectroscopy (ssNMR), Fourier-transformed infrared spectroscopy (FT-IR), Raman spectroscopy), thermal (differential scanning calorimetry (DSC), thermogravimetric analysis (TGA)), gravimetric (dynamic vapour sorption (DVS)), and computational (molecular mechanics (MM), Quantum Mechanics (QM), molecular dynamics (MD)) methods. Further, the successful applications of the presented methods in the studies of hydrated APIs as well as studies on the excipients’ influence on these processes have been described in many examples.

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.

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°.

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.

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.

Structures and physicochemical properties of vortioxetine salts

2016 ◽  
Vol 72 (5) ◽  
pp. 723-732 ◽  
Author(s):  
Xinbo Zhou ◽  
Xiurong Hu ◽  
Suxiang Wu ◽  
Jiali Ye ◽  
Mengying Sun ◽  
...  
Keyword(s):  
Antidepressant Drug ◽  
Drug Candidate ◽  
X Ray Diffraction ◽  
High Solubility ◽  
Scanning Calorimetry ◽  
Intrinsic Dissolution ◽  
X Ray ◽  
Acidic Proton ◽  
Water Ph ◽  
Ft Ir

In the present work, novel salts of the multimodal antidepressant drug vortioxetine (VT) were crystallized with pharmaceutically acceptable acids, aiming to improve the solubility of VT. The acids for VT were selected based on ΔpKabeing greater than 2 or 3. Salts of hydrobromic acid (HBr), hydrochloric acid (HCl),p-hydroxybenzoic acid (PHBA), saccharin (SAC) and L-aspartic acid (ASP) were reported. All salts were characterized by single-crystal X-ray diffraction, FT–IR, powder X-ray diffraction (PXRD) and differential scanning calorimetry (DSC). The acidic proton is transferred to the secondary N atom on the piperazine ring of VT, forming the charge-assisted hydrogen bond N+—H...X−(X= Cl, Br, O). Solubility and intrinsic dissolution rate (IDR) experiments were carried out in distilled water (pH = 7.0) to compare the solubilities of the salts with that of VT. The VT–ASP–H2O (1:1:2) salt showed 414 times higher solubility and 1722 times faster IDR compared with VT. VT–ASP–H2O (1:1:2) is a high solubility salt that is stable in a slurry experiment at 298 K in 95% ethanol. The experimental data for the VT–ASP–H2O (1:1:2) salt identify it as a promising drug candidate.

Synthesis, Characterization and Magnetism of Nanosized Copper Ferrite

2008 ◽  
Vol 368-372 ◽  
pp. 604-606 ◽  
Author(s):  
Wei Zhong Lv ◽  
Zhong Kuang Luo ◽  
Bo Liu ◽  
Xiang Zhong Ren ◽  
Hong Hua Cai ◽  
...  
Keyword(s):  
Electron Microscopy ◽  
Thermal Analysis ◽  
Copper Ferrite ◽  
Sonochemical Method ◽  
Thermal Gravimetric ◽  
X Ray Diffraction ◽  
Scanning Calorimetry ◽  
X Ray ◽  
Ft Ir ◽  
Scanning Electron

Copper ferrite powders were successfully synthesized by sonochemical method. The resultant powders were investigated by X-ray diffraction (XRD), scanning electron microscopy (SEM), FT-IR, differential thermal analysis-thermal gravimetric (DTA-TG), differential scanning calorimetry (DSC) and VSM. The particle saturation magnetization (Ms) is 66 emu/g and an intrinsic coercive force (iHc) is 2100 Oe when the precursor calcined at 950 °C for 15 h.

A New Modifier Prepared and it’s Applied in High-Density Polyethylene/Anhydrite Composites

2011 ◽  
Vol 415-417 ◽  
pp. 390-394
Author(s):  
Shao Hui Wang
Keyword(s):  
High Density Polyethylene ◽  
Bending Strength ◽  
Crystallization Rate ◽  
X Ray Diffraction ◽  
Scanning Calorimetry ◽  
X Ray ◽  
Powder Particles ◽  
Ft Ir ◽  
Anchoring Group ◽  
The Impact

A new Modifier with Silicon radicals as anchoring group and poly(butyl acrylate) as solvatable chain was synthesized and its effect on the properties of HDPE/Anhydrite composites was investigated in this paper. Fourier transmission infrared spectroscopy (FT-IR) results show that the modifier react on the Anhydrite powder particles surface and the modified Anhydrite powder particles particles. compared with that of HDPE/Anhydrite (filled with same non-modified fraction), The impact strength, tensile strength, bending strength and Young’s modulus of modified HDPE/Anhydrite composites increased about 36.6%, 7.5%, 15.6% and 34% respectively. Based on surface analysis by scanning electron microscope (SEM), the Anhydrite powder particles buried well in HDPE matrix when Anhydrite powder particles was coated with the YB modifier. It was found that Anhydrite powder particles significantly increased the crystallization temperature and crystallization rate of HDPE by differential scanning calorimetry (DSC). At same time, through the X-ray diffraction (XRD) found the addition of the YB modifier modified Anhydrite powder particles can not change the formation of crystal HDPE, but can reduce the crystallite size.

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.

Chiral Polymorphic Hydrazine-based Asymmetric Liquid Crystal Trimers with Resorcinol as Linking Group

2021 ◽  
Vol 18 ◽  
Author(s):  
Wan-Sinn Yam ◽  
Yit-Peng Goh ◽  
Foo-Win Yip ◽  
Gurumurthy Hegde
Keyword(s):  
Liquid Crystal ◽  
2D Nmr ◽  
X Ray Diffraction ◽  
Scanning Calorimetry ◽  
2D Nmr Spectroscopy ◽  
Spacer Length ◽  
X Ray ◽  
Phase Sequence ◽  
Molecular Length ◽  
Ft Ir

Introduction: This is the first report on chiral polymorphic hydrazine-based asymmetric liquid crystal trimers, 1-[4'-(4''- (5-Cholesteryloxy)carbonyl)butyloxy]-3-[N-benzylideneoxy-N'-(4'''-decyloxybenzylidene)hydrazine] butyloxybenzenes, and 1-[4'-(4''-(10-cholesteryloxy)carbonyl)nonyloxy]-3-[N-benzylideneoxy-N'-(4'''- decyloxybenzylidene)hydrazine]butyloxybenzenes., in which the hydrazine and cholesterol arms were connected via two flexible methylene spacers (n = 3-12 units and m = 4 or 9, respectively) to the central resorcinol core. Materials and Methods: FT-IR, 1D and 2D NMR spectroscopy, and CHN microanalysis were used to elucidate the structures of the trimers. Differential scanning calorimetry, polarizing optical microscopy and X-ray diffraction were used to study the transitional and phase properties of the trimers, of which they were length and spacer parity dependent. Trimers with short spacer length in the cholesteryl arm, m = 4 showed interesting phase sequence of BP/N*-TGBA*-SmA*. Results and discussion: The TGBA∗ phase was sensitive to spacer length as it was only observed in trimers with short ester linkage. For the long analogues, m = 9, characteristic visible reflection and a much simpler phase sequence with only N* and SmA* phases were seen. Conclusion: The X-ray diffraction measurements revealed that layer periodicities of the SmA* phase were approximately half the estimated all-trans molecular length (d/L ≈ 0.44-0.52), thus suggesting that the molecules are either strongly intercalated or bent.

Preparation of Nanosized Barium Ferrite Spinel by a Sonochemical Method

2008 ◽  
Vol 368-372 ◽  
pp. 607-609
Author(s):  
Bo Liu ◽  
Wei Zhong Lv ◽  
Zhong Kuang Luo ◽  
Xiang Zhong Ren ◽  
Hong Hua Cai ◽  
...  
Keyword(s):  
Electron Microscopy ◽  
Barium Ferrite ◽  
Sonochemical Method ◽  
X Ray Diffraction ◽  
Scanning Calorimetry ◽  
X Ray ◽  
Ultrasound Radiation ◽  
Ft Ir ◽  
Scanning Electron ◽  
Ferrite Spinel

Nanosized barium ferrite spinel particles were prepared with the aid of ultrasound radiation by a precursor approach. A precursor was got by sonicating an aqueous solution of BaCl2, Fe (NO3)3·9H2O and urea firstly. Nanosized BaFe2O4 particles with a size of ca.40nm were prepared after the precursor was heated at 950 °C for 15 h. The nanosized barium ferrite particles and the precursor were characterized by powder X-ray diffraction, scanning electron microscopy, FT-IR and differential scanning calorimetry.

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