New crystalline form of 7-amino-4-methylcoumarin (coumarin 120)—a polymorph with 1 ∶ 1 valence tautomers

CrystEngComm ◽  
2007 ◽  
Vol 9 (9) ◽  
pp. 735 ◽  
Author(s):  
Dorota Niedziałek ◽  
Zofia Urbanczyk-Lipkowska
Keyword(s):  
Crystalline Form ◽  
Valence Tautomers ◽  
Coumarin 120

Preparation and Properties of Human Prothrombin Complex

1970 ◽  
Vol 24 (03/04) ◽  
pp. 325-333 ◽  
Author(s):  
G. H Tishkoff ◽  
L. C Williams ◽  
D. M Brown
Keyword(s):  
Molecular Weight ◽  
Proteolytic Enzyme ◽  
Enzyme Inhibitor ◽  
Specific Activity ◽  
Crystalline Form ◽  
Sedimentation Equilibrium ◽  
Crystalline Complex ◽  
Interaction Product ◽  
Proteolytic Enzyme Inhibitor ◽  
Purification Scheme

SummaryAs a corollary to our previous studies with bovine prothrombin, we have initiated a study of human prothrombin complex. This product has been isolated in crystalline form as a barium glycoprotein interaction product. Product yields were reduced compared to bovine product due to the increased solubility of the barium glycoprotein interaction product. On occasion the crystalline complex exhibited good yields. The specific activity of the crystalline complex was 1851 Iowa u/mg. Further purification of human prothrombin complex was made by removal of barium and by chromatography on Sephadex G-100 gels. The final product evidenced multiple procoagulant activities (II, VII, IX and X). The monomeric molecular weight determined by sedimentation equilibrium in a solvent of 6 M guanidine-HCl and 0.5% mercaptoethanol was 70,191 ± 3,057 and was homogeneous with respect to molecular weight. This product was characterized in regard to physical constants and chemical composition. In general, the molecular properties of human prothrombin complex are very similar to the comparable bovine product. In some preparations a reversible proteolytic enzyme inhibitor (p-aminophenylarsonic acid) was employed in the ultrafiltration step of the purification scheme to inhibit protein degradation.

scholarly journals Combinations of Freeze-Dried Amorphous Vardenafil Hydrochloride with Saccharides as A Way to Enhance Dissolution Rate and Permeability

2021 ◽  
Vol 14 (5) ◽  
pp. 453
Author(s):  
Gabriela Wiergowska ◽  
Dominika Ludowicz ◽  
Kamil Wdowiak ◽  
Andrzej Miklaszewski ◽  
Kornelia Lewandowska ◽  
...  
Keyword(s):  
Physicochemical Properties ◽  
Density Functional ◽  
Hydroxypropyl Methylcellulose ◽  
Fold Increase ◽  
Crystalline Form ◽  
Amorphous Form ◽  
Freeze Dried ◽  
Apparent Solubility ◽  
Gastrointestinal Epithelium ◽  
The Impact

To improve physicochemical properties of vardenafil hydrochloride (VAR), its amorphous form and combinations with excipients—hydroxypropyl methylcellulose (HPMC) and β-cyclodextrin (β-CD)—were prepared. The impact of the modification on physicochemical properties was estimated by comparing amorphous mixtures of VAR to their crystalline form. The amorphous form of VAR was obtained as a result of the freeze-drying process. Confirmation of the identity of the amorphous dispersion of VAR was obtained through the use of comprehensive analysis techniques—X-ray powder diffraction (PXRD) and differential scanning calorimetry (DSC), supported by FT-IR (Fourier-transform infrared spectroscopy) coupled with density functional theory (DFT) calculations. The amorphous mixtures of VAR increased its apparent solubility compared to the crystalline form. Moreover, a nearly 1.3-fold increase of amorphous VAR permeability through membranes simulating gastrointestinal epithelium as a consequence of the changes of apparent solubility (Papp crystalline VAR = 6.83 × 10−6 cm/s vs. Papp amorphous VAR = 8.75 × 10−6 cm/s) was observed, especially for its combinations with β-CD in the ratio of 1:5—more than 1.5-fold increase (Papp amorphous VAR = 8.75 × 10−6 cm/s vs. Papp amorphous VAR:β-CD 1:5 = 13.43 × 10−6 cm/s). The stability of the amorphous VAR was confirmed for 7 months. The HPMC and β-CD are effective modifiers of its apparent solubility and permeation through membranes simulating gastrointestinal epithelium, suggesting a possibility of a stronger pharmacological effect.

Observation of Discrete Valence Tautomers in Crystalline Cyclopentadienyl Radicals

2021 ◽  
Author(s):  
Yannick Schulte ◽  
Blaise L. Geoghegan ◽  
Christoph Helling ◽  
Christoph Wölper ◽  
Gebhard Haberhauer ◽  
...  
Keyword(s):  
Valence Tautomers

Syntheses related to the carbohydrate moiety in lincomycin

1969 ◽  
Vol 47 (1) ◽  
pp. 75-79 ◽  
Author(s):  
G. B. Howarth ◽  
D. G. Lance ◽  
W. A. Szarek ◽  
J. K. N. Jones
Keyword(s):  
Crystalline Form ◽  
Carbohydrate Moiety ◽  
Allylic Alcohols ◽  
Nitro Derivatives ◽  
Sugar Derivatives ◽  
Cis And Trans

Addition of nitroethane to 1,2:3,4-di-O-isopropylidene-α-D-galacto-hexodialdo-1,5-pyranose (3) gave a mixture of β-nitro alcohols (4), which was acetylated to afford a mixture of β-nitro acetates (5). Dehydroacetylation of the latter gave cis- and trans-6,7,8-trideoxy-1,2:3,4-di-O-isopropylidene-7-C-nitro-α-D-galacto-oct-6-enose (6 and 7) in a ratio of about 6:1, respectively. Addition of ammonia to the cis-nitroolefin (6) gave rapidly a mixture of two stereoisomeric vic-nitroamines (8), which was acetylated to furnish a mixture of two 6-acetamido-6,7-dideoxy-7-C-nitro derivatives (9). The same products (9) were obtained by the action of ammonia in aqueous tetrahydrofuran upon the preponderant β-nitro acetate, followed by acetylation. Vinylation of the aldehyde 3 gave a mixture of allylic alcohols (10); the preponderant epimer was obtained pure in crystalline form. The various 8-carbon sugar derivatives are of interest as potential intermediates in the synthesis of the carbohydrate moiety in lincomycin.

Preparation and Characterization of Ni-Containing Aluminophosphate Molecular Sieves

2011 ◽  
Vol 418-420 ◽  
pp. 617-620
Author(s):  
Ying Sun ◽  
Lan Ying Ge
Keyword(s):  
Oxidation State ◽  
Molecular Sieves ◽  
Molecular Sieve ◽  
Crystalline Form ◽  
Spectroscopic Techniques ◽  
Tetrahedral Coordination ◽  
Tetrahedral Geometry ◽  
Nickel Ions ◽  
Aluminophosphate Molecular Sieves

Aluminophosphate molecular sieve and Ni(II)-containing APO-5 materials were synthesized hydrothermally and characterized by various analytical and spectroscopic techniques. It indicates that the nickel ions with a divalent oxidation state can incorporate into the tetrahedral coordination in mesoporous aluminophosphate very well. The better crystallizing temperature is explored. A stronger crystalline form is obtained with the addition of HF. Further, microporous aluminophosphate molecular sieves and Ni(II) ions remain in a tetrahedral geometry even after calcination at 550 °C.

scholarly journals Characterization of hydrochlorothiazide in solid formulations

2015 ◽  
Vol 30 (S1) ◽  
pp. S127-S130
Author(s):  
Simone T. B. de Salvi ◽  
Diego Luiz Tita ◽  
Carlos de O. Paiva-Santos ◽  
Selma G. Antonio
Keyword(s):  
Rietveld Method ◽  
Package Insert ◽  
Polymorphic Form ◽  
Crystalline Form ◽  
Active Principle ◽  
Lauryl Sulfate ◽  
X Ray ◽  
Lactose Monohydrate ◽  
Solid State Characterization

Hydrochlorothiazide (HCTZ) is a diuretic used for the treatment of blood pressure (hypertension). HCTZ has two anhydrous polymorphs denoted as Forms I and II. Aiming at solid-state characterization, X-ray powder diffraction (XRPD) is known to be a powerful technique which has been successfully applied in investigating polymorphism in medicines. In this work, three tablets of HCTZ (a reference and two generic) were analyzed. The data were collected using Rigaku RINT2000 diffractometer copper rotate anode. The Rietveld method (RM) was applied for the characterization of HCTZ polymorphic form. For the crystalline excipients where the crystal structure is known, their phases were identified by the RM either. The results showed that all the tablets exhibit Form I of HCTZ, while the excipient lactose monohydrate is found to exhibit the crystalline form. One of the generics is also found to exhibit the excipient sodium lauryl sulfate (SLS) in the crystalline form. Therefore, the RM and XRPD are an efficient methodology for characterization of the crystalline Form I of the active principle of HCTZ and crystalline excipients lactose monohydrate and SLS in solid formulations. It is also interesting to observe excipients not described in the package insert of the medicament.

scholarly journals Purification and properties of two extracellular β-lactamases from Bacillus cereus 569/H

1970 ◽  
Vol 118 (3) ◽  
pp. 457-465 ◽  
Author(s):  
S. Kuwabara
Keyword(s):  
Molecular Weight ◽  
Bacillus Cereus ◽  
Zinc Sulphate ◽  
Deae Cellulose ◽  
Casein Hydrolysate ◽  
Crystalline Form ◽  
Casamino Acid ◽  
Fractional Precipitation ◽  
Purification And Properties ◽  
Rapid Production

1. When Bacillus cereus 569/H was grown in a casamino acid (casein-hydrolysate) medium containing zinc sulphate rapid production of extracellular β-lactamase II preceded that of β-lactamase I. 2. β-Lactamase I was separated from β-lactamase II by fractional precipitation with ammonium sulphate. 3. β-Lactamase I was purified by a process involving chromatography on Celite and DEAE-cellulose and β-lactamase II by chromatography on DEAE-cellulose after denaturation of β-lactamase I by heat. Both enzymes were obtained in crystalline form. 4. β-Lactamase II prepared in this way appeared to have a higher molecular weight than β-lactamase I and required Zn2+ as a cofactor for both cephalosporinase and penicillinase activities.

Prostaglandin E and the Ductus Arteriosus

1985 ◽  
Vol 7 (3) ◽  
pp. 75-76
Keyword(s):  
Smooth Muscle ◽  
Seminal Fluid ◽  
Ductus Arteriosus ◽  
Active Material ◽  
Crystalline Form ◽  
Prostaglandin E ◽  
Chemical Structures ◽  
Soluble Acid ◽  
Derivatives Of ◽  
Widespread Interest

In 1936, Euler of Sweden identified in seminal fluid an active material that contracts smooth muscle; he named this lipid-soluble acid "prostaglandin." More than 20 years passed before the isolation in crystalline form of two prostaglandins, PGE1 and PGE1a, was accomplished. The elucidation of their chemical structures in 1962 by Bergstrom led to their biosynthesis in 1964. Few substances have generated more widespread interest in biologic circles than the prostaglandins. The prostaglandins are derivatives of fatty acids and have been detected in almost every tissue including the fetal ductus. The E-type prostaglandins are powerful vasodilators of nearly all arterioles by direct relaxation of vascular smooth muscle.

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