scholarly journals Physical Mixture Interaction of Acetaminophenol with Naringenin

2018 ◽  
Vol 18 (1) ◽  
pp. 18 ◽  
Author(s):  
Normyzatul Akmal Abd Malek ◽  
Hamizah Mohd Zaki ◽  
Mohammad Noor Jalil
Keyword(s):  
Interaction Strength ◽  
Active Pharmaceutical Ingredient ◽  
Binary Interaction ◽  
Molar Ratio ◽  
Attenuated Total Reflectance ◽  
X Ray Diffraction ◽  
Scanning Calorimetry ◽  
Mixture Ratio ◽  
X Ray ◽  
New Phase

The interaction of Active Pharmaceutical Ingredient (API) with other compounds will affect drugs stability, toxicity, modified dissolution profiles or may form a new compound with the different crystal structure. Acetaminophenol (APAP), the most common drug used widely (also known as Panadol) was mixed with Naringenin (NR) to glance for a new phase of interactions leading to new compound phase. The amide-acid supramolecular heterosynthon; N-H…O interaction between acid and the respective base were observed in the APAP-NR mixture blends. The interaction was prepared by the binary interaction from neat grinding and liquid-assisted grinding techniques at a different stoichiometry of binary mixture ratio of APAP-NR which were 1:1, 1:2 and 2:1 molar ratio. The interaction was estimated using Group Contribution Method (GCM) and physicochemical properties were characterized by Attenuated Total Reflectance Fourier Transform Infrared (ATR-FTIR), powder X-ray diffraction (PXRD) and Differential Scanning Calorimetry (DSC) analysis. The GCM calculation gave good interaction strength at 212.93 MPa1/2. The ATR-FTIR, DSC and PXRD results obtained revealed an interaction with new phase formed.

scholarly journals Microstructure Evolution and Performance Improvement of Hypereutectic Al–Mg2Si Metallic Composite with Ca or Sb

Materials ◽  
2020 ◽  
Vol 13 (12) ◽  
pp. 2714
Author(s):  
Min Zuo ◽  
Boda Ren ◽  
Zihan Xia ◽  
Wenwen Ma ◽  
Yidan Lv ◽  
...  
Keyword(s):  
Heat Treatment ◽  
Molar Ratio ◽  
X Ray Diffraction ◽  
Scanning Calorimetry ◽  
Nucleation Behavior ◽  
X Ray ◽  
Primary Mg2si ◽  
Before And After ◽  
And Performance ◽  
Hardness Values

In this article, the modification effects on Al–Mg2Si before and after heat treatment were investigated with Ca, Sb, and (Ca + Sb). In comparison with single Ca or Sb, the samples with composition modifiers (Ca + Sb) had the optimal microstructure. The sample with a molar ratio for Ca-to-Sb of 1:1 obtained relatively higher properties, for which the Brinell hardness values before and after heat treatment were remarkably increased by 31.74% and 28.93% in comparison with bare alloy. According to differential scanning calorimetry analysis (DSC), it was found that the nucleation behavior of the primary Mg2Si phase could be significantly improved by using chemical modifiers. Some white particles were found to be embedded in the center of Mg2Si phases, which were deduced to be Ca5Sb3 through X-ray diffraction (XRD) and field-emission scanning electron microscope (FESEM) analyses. Furthermore, Ca5Sb3 articles possess a rather low mismatch degree with Mg2Si particles based on Phase Transformation Crystallography Lab software (PTCLab) calculation, meaning that the efficient nucleation capability of Ca5Sb3 for Mg2Si particles could be estimated.

scholarly journals Compression-Induced Phase Transitions of Bicalutamide

Pharmaceutics ◽  
2020 ◽  
Vol 12 (5) ◽  
pp. 438 ◽  
Author(s):  
Joanna Szafraniec-Szczęsny ◽  
Agata Antosik-Rogóż ◽  
Justyna Knapik-Kowalczuk ◽  
Mateusz Kurek ◽  
Ewa Szefer ◽  
...  
Keyword(s):  
Solid Dispersions ◽  
Amorphous Solid ◽  
Active Pharmaceutical Ingredient ◽  
X Ray Diffraction ◽  
Scanning Calorimetry ◽  
Amorphous Solid Dispersions ◽  
X Ray ◽  
High Propensity ◽  
Poorly Soluble ◽  
Amorphous Drug

The formation of solid dispersions with the amorphous drug dispersed in the polymeric matrix improves the dissolution characteristics of poorly soluble drugs. Although they provide an improved absorption after oral administration, the recrystallization, which can occur upon absorption of moisture or during solidification and other formulation stages, serves as a major challenge. This work aims at understanding the amorphization-recrystallization changes of bicalutamide. Amorphous solid dispersions with poly(vinylpyrrolidone-co-vinyl acetate) (PVP/VA) were obtained by either ball milling or spray drying. The applied processes led to drug amorphization as confirmed using X-ray diffraction and differential scanning calorimetry. Due to a high propensity towards mechanical activation, the changes of the crystal structure of physical blends of active pharmaceutical ingredient (API) and polymer upon pressure were also examined. The compression led to drug amorphization or transition from form I to form II polymorph, depending on the composition and applied force. The formation of hydrogen bonds confirmed using infrared spectroscopy and high miscibility of drug and polymer determined using non-isothermal dielectric measurements contributed to the high stability of amorphous solid dispersions. They exhibited improved wettability and dissolution enhanced by 2.5- to 11-fold in comparison with the crystalline drug. The drug remained amorphous upon compression when the content of PVP/VA in solid dispersions exceeded 20% or 33%, in the case of spray-dried and milled systems, respectively.

scholarly journals Synthesis of Glibenclamide-Oxalic Acid Cocrystal using ThermalSolvent-Free Method

2020 ◽  
Vol 11 (03) ◽  
pp. 404-408
Author(s):  
Arif Budiman ◽  
Sandra Megantara ◽  
Rifaa’tush Sholihah ◽  
Saeful Amin
Keyword(s):  
Oxalic Acid ◽  
In Silico ◽  
Active Pharmaceutical Ingredient ◽  
Molar Ratio ◽  
Dissolution Profile ◽  
X Ray Diffraction ◽  
Scanning Calorimetry ◽  
Dissolution Tests ◽  
Ir Spectrophotometry ◽  
Crystalline Component

Solubility is an important parameter affecting the bioavailability of drugs. The solubility of an active pharmaceutical ingredient (API) could be improved through the formation of cocrystal, which is a crystalline complex composed of two or more different molecules. Glibenclamide (GCM) is an API with poor solubility in water, which belongs to class II, characterized as highly permeable with low solubility. Therefore, this study aimed to synthesize and characterize the cocrystal of GCM-oxalic acid (OA) using the melting method. The interaction between GCM-OA complexes was predicted using the in silico method. Also, the cocrystal complexes were characterized by differential scanning calorimetry (DSC), infrared (IR) spectrophotometry, and powder X-ray diffraction (PXRD), as well as, through solubility and dissolution tests. The result showed that GCM and OA have the potential of forming cocrystal through the in silico method. Also, the cocrystal of GCM-OA with a molar ratio 1:2, significantly improved the solubility and dissolution profile of GCM. In addition, the spectrum IR of cocrystal exhibited a shifting peak at 1,700 cm-1 indicating the presence of intermolecular interaction between GCM and OA. Furthermore, the DSC and PXRD analyses showed a new single endothermic peak and new diffraction peak pattern, respectively, indicating the formation of a new crystalline component.

Structural and Mechanical Properties of Nanostructured Fe-Mn-C Alloys Prepared by Mechanical Alloying

2018 ◽  
Vol 52 ◽  
pp. 80-87 ◽  
Author(s):  
Lounes Belaid ◽  
Meriem Bendoumia ◽  
Mohamed Dakiche ◽  
Hanane Mechri ◽  
Djaffar Dahmoun ◽  
...  
Keyword(s):  
Milling Time ◽  
Milled Powder ◽  
Nanocrystalline Structure ◽  
Hadfield Steel ◽  
X Ray Diffraction ◽  
Scanning Calorimetry ◽  
X Ray ◽  
Grain Sizes ◽  
New Phase ◽  
High Manganese Austenitic Steel

The object of our research is to combine the properties of Mangalloys and nanoscale advantages in order to enhance the performance and extend the range of applications in the field of work-hardening parts such as railroad components, armor, and modern auto components. We have produced a high-manganese austenitic steel nanomaterial containing more than 12 wt% Mn, which is the level of Mn in Hadfield steel. This study experimentally determined the process of phase transitions involved in Fe–13 wt% Mn–1.2 wt% C alloy during mechano-synthesis and after subsequent annealing. The milling time ranged from 0.5 to 24 h. The unique features of the nanocrystalline structure and the changes in microstructure as a function of milling time were investigated by X-ray diffraction analysis, differential scanning calorimetry, and scanning electron microscopy coupled with EDX. The grain sizes and microstrain of the milled powder were determined. A thorough study has been done on the sample where a new phase fcc (at 24h of MA) was formed.The object of our research is to combine the properties of Mangalloys and nanoscale advantages in order to enhance the performance and extend the range of applications in the field of work-hardening parts such as railroad components, armor, and modern auto components. We have produced a high-manganese austenitic steel nanomaterial containing more than 12 wt% Mn, which is the level of Mn in Hadfield steel. This study experimentally determined the process of phase transitions involved in Fe–13 wt% Mn–1.2 wt% C alloy during mechano-synthesis and after subsequent annealing. The milling time ranged from 0.5 to 24 h. The unique features of the nanocrystalline structure and the changes in microstructure as a function of milling time were investigated by X-ray diffraction analysis, differential scanning calorimetry, and scanning electron microscopy coupled with EDX. The grain sizes and microstrain of the milled powder were determined. A thorough study has been done on the sample where a new phase fcc (at 24h of MA) was formed.

scholarly journals Pengaruh Bentonit terhadap Pembentukan Fasa Polimorf dan Sifat Termal Membran Hibrida Poliviniliden Fluorida/Bentonit

2021 ◽  
Vol 17 (2) ◽  
pp. 177
Author(s):  
Edi Pramono ◽  
Rosid Eka Mustofa ◽  
Ozi Adi Saputra ◽  
Yulianto Adi Nugroho ◽  
Deana Wahyunigrum ◽  
...  
Keyword(s):  
Differential Scanning Calorimetry ◽  
Fourier Transform ◽  
Thermal Properties ◽  
Phase Formation ◽  
Attenuated Total Reflectance ◽  
Hybrid Membranes ◽  
X Ray Diffraction ◽  
Scanning Calorimetry ◽  
Total Reflectance ◽  
X Ray

<p>Kajian struktur dan degradasi termal pada membran hibrida poliviniliden fluorida (PVDF)/lempung bentonit (BNT) telah dilakukan. Penelitian ini bertujuan mengetahui pengaruh penambahan BNT terhadap pembentukan fasa PVDF dan sifat termalnya. Membran hibrida PVDF/lempung BNT dibuat dengan metode inversi fasa. Membran yang dihasilkan dikarakterisasi dengan <em>attenuated total reflectance fourier transform infrared</em> (ATR-FTIR), <em>x-ray diffraction</em> (XRD), dan <em>differential scanning calorimetry</em> (DSC). Hasil penelitian menunjukkan membran PVDF/BNT memiliki struktur polimorf PVDF fasa α dan β yang terkonfirmasi dari data FTIR dan XRD. Data DSC menunjukkan penurunan nilai titik leleh (Tm) dengan penambahan BNT, dan dengan rentang suhu pelelehan yang lebih kecil. Kristalisasi PVDF terjadi secara isothermal dan adanya BNT menghasilkan titik kristalisasi (Tc) pada suhu yang lebih tinggi dibandingkan membran PVDF murni. Analisis termal dengan DSC memberikan informasi komprehensif pelelehan dan kristalisasi dari polimorf PVDF pada matriks membran.</p><p id="docs-internal-guid-c92edf53-7fff-cf03-76f3-f207f37c74f5" style="line-height: 1.2; text-align: justify; margin-top: 6pt; margin-bottom: 6pt;" dir="ltr"><strong>Effect of Bentonite toward Polymorph Phase Formation and Thermal Properties of Polyvinylidene Fluoride/Bentonite Hybrid Membranes. </strong>The study of the structure and thermal properties of PVDF/bentonite (BNT) hybrid membranes has been carried out. This study aims to determine the effect of BNT addition on the phase formation and thermal properties of the PVDF. In this study, PVDF/BNT hybrid membranes were prepared through the phase inversion method. The resulting membrane was characterized by Attenuated Total Reflectance Fourier Transform Infrared (ATR-FTIR), x-ray diffraction (XRD), and differential scanning calorimetry (DSC). The results showed that the PVDF/BNT membrane has a PVDF polymorph structure with α and β phases confirmed by FTIR and XRD data. The DSC data showed that the addition of BNT decrease of the melting point (Tm) and with a smaller melting temperature range. PVDF polymorph crystallization occurs isothermally and the presence of BNT produces a crystallization point (Tc) at a higher temperature than pristine PVDF membrane. Thermal analysis with DSC provides comprehensive information on melting and crystallization of PVDF polymorphs in the membrane matrix.</p>

scholarly journals Effect of Calcination on Shell Powder Catalyst Towards Effectiveness on Catalysing Transesterification of Crude Glycerol to Glycerol Carbonate

2021 ◽  
Vol 945 (1) ◽  
pp. 012038
Author(s):  
Janice Sheow Tung Liew ◽  
Siew Yong Leong ◽  
Po Kim Lo
Keyword(s):  
Crude Glycerol ◽  
Dimethyl Carbonate ◽  
Molar Ratio ◽  
Attenuated Total Reflectance ◽  
Glycerol Carbonate ◽  
Base Catalyst ◽  
X Ray Diffraction ◽  
Total Reflectance ◽  
X Ray ◽  
Shell Powder

Abstract Valorisation of crude glycerol has gained much interest in the industry associated with the surplus of crude glycerol caused by the increase usage of biodiesel. Transesterification of crude glycerol using a heterogenous base catalyst is one of the effective ways to utilize the additional glycerol. Seawater clams commonly serve as a food source to us and the waste shells are a source of calcium carbonate that is abundantly available and can be converted into a heterogenous base catalyst for the transesterification process. Therefore, this study focuses on the utilization of catalyst synthesized from a species of seawater clam, Paratapes Undulatus in a transesterification reaction using crude glycerol (C.GLY) as a reactant together with dimethyl carbonate (DMC) to synthesize glycerol carbonate (GLYC). The catalysts are characterized using Field Emission Scanning Electron Microscope (FESEM), Attenuated Total Reflectance (ATR), Thermogravimetric Analysis (TGA), X-ray diffraction (XRD) and Particle Size Analyser (PSA). The product is characterized using Gas Chromatography (GC-FID). The performance of the synthesized shell catalyst with different calcination condition was studied. The reaction using the calcined shell catalyst is carried out at 75°C, molar ratio of 2 and 2wt% of catalyst for 1 hour. The catalyst that has the best performance is the shell catalyst that is calcined for 3h, which give the yield of 54.16%.

Co-Amorphous Telmisartan-Pimelic Acid with Improved Solubility

2020 ◽  
Vol 993 ◽  
pp. 776-784
Author(s):  
Ze Xin Wu ◽  
Wen Zhe Ma ◽  
Lei Wang ◽  
Chang Lin Yao ◽  
Shuang Song ◽  
...  
Keyword(s):  
Differential Scanning Calorimetry ◽  
Infrared Spectra ◽  
Molar Ratio ◽  
Pimelic Acid ◽  
X Ray Diffraction ◽  
Scanning Calorimetry ◽  
X Ray ◽  
Amorphous System ◽  
Grinding Method ◽  
Apparent Solubility

Telmisartan (TEL), a type of antihypertensive drug, has poor solubility. To improve its solubility, the co-amorphous telmisartan with pimelic acid (PA) in molar ratio of 1:1 and 2:1, respectively, were obtained using a liquid-assisted grinding method. The co-amorphous system was characterized by the powder X-ray diffraction and differential scanning calorimetry. The molecular interactions of the co-amorphous were studied by the infrared spectra. After the formation of co-amorphous, the solubility of TELwas much improved, and the apparent solubility values were approximately 9-15 times as high as that of crystalline TEL. Moreover, the co-amorphous TEL-PA was stored under 25 °C/20% RH for a month without any evidence of conversion by powder X-ray diffraction analysis.

scholarly journals Systematic synthesis of a 6-component organic-salt alloy of naftopidil, and pentanary, quaternary and ternary multicomponent crystals

IUCrJ ◽  
2018 ◽  
Vol 5 (6) ◽  
pp. 816-822 ◽  
Author(s):  
Rambabu Dandela ◽  
Srinu Tothadi ◽  
Udaya Kiran Marelli ◽  
Ashwini Nangia
Keyword(s):  
Single Crystal ◽  
Carboxylic Acids ◽  
Active Pharmaceutical Ingredient ◽  
Organic Salt ◽  
X Ray Diffraction ◽  
Dihydroxybenzoic Acid ◽  
Scanning Calorimetry ◽  
Organic Salts ◽  
X Ray ◽  
Substituted Benzoic Acids

The single-crystal X-ray structure of a 6-component organic-salt alloy (hexanary) of naftopidil (1) (an active pharmaceutical ingredient) with benzoic acid (2) and four different hydroxy-substituted benzoic acids, i.e. salicylic acid (3), 2,3-dihydroxybenzoic acid (4), 2,4-dihydroxybenzoic acid (5) and 2,6-dihydroxybenzoic acid (6), is reported. The hexanary assembly originates from the observation that the binary salts of naftopidil with the above acids are isostructural. In addition to the 6-component solid, we also describe five 5-component, ten 4-component, and ten 3-component organic-salt alloys of naftopidil (1) with carboxylic acids (2)–(6). These alloys were obtained from different combinations of the acids with the drug. The synthetic design of the multicomponent organic alloys is based on the rationale of geometrical factors (shape and size) and chemical interactions (hydrogen bonds). The common supramolecular synthon in all these crystal structures was the cyclic N+—H...O− and O—H...O hydrogen-bonded motif of R_2^2(9) graph set between the 2-hydroxyammonium group of naftopidil and the carboxylate anion. This ionic synthon is strong and robust, directing the isostructural assembly of naftopidil with up to five different carboxylic acids in the crystal structure together with the lower-level multicomponent adducts. Solution crystallization by slow evaporation provided the multicomponent organic salts and alloys which were characterized by a combination of single-crystal X-ray diffraction, powder X-ray diffraction, NMR and differential scanning calorimetry techniques.

scholarly journals Facile Synthesis of Mn0.68Bi0.32OCl Mix-Crystals And Its Supercapacitive Behavior

2021 ◽  
Author(s):  
Y.Z. Song ◽  
B.X. Qi ◽  
M.T. Li ◽  
J.M. Xie
Keyword(s):  
Surface Area ◽  
Solid Phase ◽  
Life Time ◽  
Molar Ratio ◽  
Phase Method ◽  
X Ray Diffraction ◽  
Facile Synthesis ◽  
Scanning Calorimetry ◽  
X Ray ◽  
Solid Phase Method

Abstract Mn0.68Bi0.32OCl mix-crystals for supercapacitor were successfully synthesized via a facile solid-phase method using Bi(NO3)3 and MnCl2 with molar ratio of 1:1 as precursors. The Mn0.68Bi0.32OCl mix-crystals were characterized by scanning electron microscopy, X-ray diffraction, Brunauer-Emmett-Teller surface area measurements and thermogravimetry and differential scanning calorimetry, respectively. Cyclic voltammetry and galvanostatic charge/discharge technique were performed for the Mn0.68Bi0.32OCl mix-crystals in 1 M Na2SO4 aqueous solutions; the specific capacitance of Mn0.68Bi0.32OCl was about 203 F.g-1 at the current density of 3 A. g-1 with a long life time, owing to the high power density of Mn0.68Bi0.32OCl mix-crystals and the higher surface area, good conductivity, and high stability of the Mn0.68Bi0.32OCl mix-crystals.

The synthesis of novel polynuclear organogold complexes

1998 ◽  
Vol 546 ◽  
Author(s):  
J. Thomson ◽  
A. H. Fzea ◽  
J. Lobban ◽  
P. G. McGivern ◽  
J. A. Cairns ◽  
...  
Keyword(s):  
Deposition Process ◽  
Molar Ratio ◽  
Gold Content ◽  
X Ray Diffraction ◽  
Scanning Calorimetry ◽  
X Ray ◽  
Atomic Force ◽  
Scanning Transmission ◽  
Physical And Chemical ◽  
Characterisation Methods

SummaryThe synthesis and peirastic characterisation of two new organogold(III) complexes with a high molar ratio of gold content is described. The proposed formulae for the complexes in the present study are [C2H2Au4F8(PPh3)4]n and [C2H2Au4F8(NCCH3)4]n (Figure 1). These complexes were found to be stable to the atmosphere. The aim of this work was to demonstrate that such materials have a high metal to ligand ratio, suitable for physical vapour deposition process (PVD) and, hence, can be used as precursors for the deposition of pure metallic features. Physical and chemical characterisation methods were employed to obtain information about i) the structures, ii) the thermal and chemical stability, iii) the volatility and iv) the adhesion of these materials to specific substrates. These include n.m.r. (1H, 19F, 13C and 31P) IR spectroscopy, EDX (Energy Dispersive X-ray analysis), DSC ( Differential Scanning Calorimetry), TGA (Thermogravimetric Analysis), Powder X-ray Diffraction and Electron Microscopy (Scanning, Transmission and Atomic Force).

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