ISOLATION OF CRYSTALLINE 16-EPIESTRIOL FROM HEN URINE

1964 ◽  
Vol 42 (8) ◽  
pp. 1177-1182 ◽  
Author(s):  
F. Hertelendy ◽  
R. H. Common
Keyword(s):  
Crystalline Form ◽  
Chromatographic Behavior ◽  
Melting Points ◽  
Solvent Systems

16-Epiestriol has been isolated in crystalline form from hen urine and characterized on the basis of the melting points of the isolated product and of two of its derivatives (acetonide, triacetate) and on the chromatographic behavior of the isolated product and five of its derivatives in each of three different solvent systems.

scholarly journals THE CHEMISTRY OF THE "AMINOCHROMES": PART I. THE PREPARATION AND PAPER CHROMATOGRAPHY OF PURE ADRENOCHROME

1958 ◽  
Vol 36 (5) ◽  
pp. 853-857 ◽  
Author(s):  
R. A. Heacock ◽  
C. Nerenberg ◽  
A. N. Payza
Keyword(s):  
Heavy Metal Ions ◽  
Silver Oxide ◽  
Exchange Resin ◽  
Anion Exchange Resin ◽  
Acid Hydrazide ◽  
Crystalline Form ◽  
Chromatographic Behavior ◽  
Mixture Prior ◽  
Solvent Systems ◽  
Dowex 1

The preparation of adrenochrome in a pure stable crystalline form has been carried out by the silver oxide oxidation of adrenaline in methanol with the use of an anion-exchange resin (Dowex-1(Cl−)) to remove heavy metal ions from the reaction mixture prior to the isolation of the product. Its paper chromatographic behavior together with that of three derivatives (adrenolutin, adrenochrome monosemicarbazone, and adrenochrome monoisonicotinic acid hydrazide) in six different solvent systems has been examined. Water was found to be the best paper chromatographic solvent so far examined for this series of compounds.

ISOLATION OF ESTRADIOL-17β FROM HEN'S URINE AND ITS CHARACTERIZATION AS THE CRYSTALLINE 3-METHYL ETHER

1965 ◽  
Vol 43 (9) ◽  
pp. 1379-1385 ◽  
Author(s):  
F. Hertelendy ◽  
T. G. Taylor ◽  
R. S. Mathur ◽  
R. H. Common
Keyword(s):  
Melting Point ◽  
Thin Layer ◽  
Methyl Ether ◽  
Crystalline Form ◽  
Crystalline Material ◽  
Chromatographic Behavior ◽  
Estradiol 17Β

Estradiol-17β-3-methyl ether has been prepared in crystalline form from the phenolic steroid fraction of hen's urine and characterized by its melting point, the melting point of its acetate, and the chromatographic behavior of the crystalline material, of its acetate, and of its benzoate in each of three different thin-layer chromatographic systems.The method of Brown has been modified to render it more specific for the determination of estradiol-17β in hen's urine. Values for the estradiol-17β content of the urine of laying and nonlaying hens are reported.

Purification and partial characterization of an antibiotic produced by Myxococcus xanthus

1974 ◽  
Vol 20 (2) ◽  
pp. 155-161 ◽  
Author(s):  
B. Vaks ◽  
A. Zuckerberg ◽  
E. Rosenberg
Keyword(s):  
Mass Spectra ◽  
Protein Hydrolysate ◽  
Antibiotic Production ◽  
Myxococcus Xanthus ◽  
Chromatographic Behavior ◽  
Gram Negative Bacteria ◽  
Apparent Homogeneity ◽  
Silicic Acid Chromatography ◽  
Solvent Systems

A strain of Myxococcus xanthus, referred to as M. xanthus TA, has been isolated which produces an antibiotic capable of inhibiting growth of certain Gram-positive and Gram-negative bacteria. Antibiotic production was significantly inhibited when the concentration of protein hydrolysate in the production medium exceeded 1%. The antibiotic was purified over 1000 times to apparent homogeneity by silicic acid chromatography and by a variety of preparative alumina thin-layer chromatographic procedures. The purified antibiotic was partially characterized by its chromatographic behavior in six solvent systems, stability to acid, alkali and heat, infrared, ultraviolet, and mass spectra. The antibiotic has a λmax of 242 nm in methanol.

Non-equilibrium freezing behaviour of aqueous systems

1977 ◽  
Vol 278 (959) ◽  
pp. 167-189 ◽  
Keyword(s):  
Heterogeneous Nucleation ◽  
Homogeneous Nucleation ◽  
Living Cells ◽  
Crystalline Form ◽  
Model Systems ◽  
Aqueous Systems ◽  
Melting Points ◽  
Simultaneous Representation ◽  
Thermodynamic Factors ◽  
Non Equilibrium

The tendencies to non-equilibrium freezing behaviour commonly noted in representative aqueous systems derive from bulk and surface properties according to the circumstances. Supercooling and supersaturation are limited by heterogeneous nucleation in the presence of solid impurities. Homogeneous nucleation has been observed in aqueous systems freed from interfering solids. Once initiated, crystal growth is often slowed and, very frequently, terminated with increasing viscosity. Nor does ice first formed always succeed in assuming its most stable crystalline form. Many of the more significant measurements on a given system can be combined and displayed in the form of a ‘supplemented phase diagram’, the latter permitting the simultaneous representation of thermodynamic and non-equilibrium properties. The diagram incorporates equilibrium melting points, heterogeneous nucleation temperatures, homogeneous nucleation temperatures, glass transition and devitrification temperatures, recrystallization temperatures, and, where appropriate, solute solubilities and eutectic temperatures. Taken together, the findings on model systems aid the identification of the kinetic and thermodynamic factors responsible for the freezing - thawing survival of living cells.

Thin Layer Chromatographic Identification of Some Sympathomimetic Amines

1976 ◽  
Vol 59 (6) ◽  
pp. 1416-1418
Author(s):  
Jitendra J Shah ◽  
Ramila J Shah
Keyword(s):  
Organic Solvent ◽  
Thin Layer ◽  
Ethyl Acetate ◽  
Solvent System ◽  
Chromatographic Behavior ◽  
Bromocresol Green ◽  
Sympathomimetic Amines ◽  
Solvent Systems ◽  
Glass Plates

Abstract Thin layer chromatographic behavior of some sympathomimetic amines in the presence of acids in neutral and organic solvent systems is reported. The sympathomimetic amines were dissolved in 0.1N HCl or ethanol and treated with bromocresol green or p-nitrobenzoyl chloride reagents on fiber sheets or precoated glass plates. Two-, 3-, and 4-component solvent systems were tested. Benzene-ethyl acetate gave 2 spots for each amine standard; the more polar spots were satisfactorily separated. Amines in pharmaceuticals were not separated by any solvent system tested.

An in-situ high-temperature structural study of stable and metastable CaAl2Si2O8 polymorphs

1995 ◽  
Vol 59 (394) ◽  
pp. 25-33 ◽  
Author(s):  
I. Daniel ◽  
P. Gillet ◽  
P. F. McMillan ◽  
P. Richet
Keyword(s):  
Raman Spectroscopy ◽  
High Temperature ◽  
Liquidus Temperature ◽  
Hexagonal Phase ◽  
Crystalline Form ◽  
Melting Points ◽  
Actual Structure ◽  
Alumino Silicate ◽  
Silicate Framework

AbstractHigh-temperature Raman spectroscopy and optical microscopic observations have revealed a new metastable polymorph of CaAl2Si2O8 composition, which brings to four the number of known crystalline phases in this system. Similar to the metastable monoclinic pseudo-orthorhombic and pseudo-hexagonal phases, the new polymorph nucleates prior to anorthite, at around 1545 K, and its pseudo-liquidus temperature is 1700 ± 10 K. It can also be formed from the transformation of the pseudo-hexagonal phase at 1050 K. The actual structure of this new crystalline form is unknown, but its Raman spectrum indicates that it is most likely a 6-membered alumino-silicate framework. We have obtained all three metastable phases as pure single crystals using wire loop heating techniques, and have studied their structures via Raman spectroscopy up to their metastable melting points or transformation temperatures.

THE PREPARATION AND PROPERTIES OF THE POTASSIUM SKATOLYL SULFATES (THE "SULFATOXYSKATOLES")

1965 ◽  
Vol 43 (4) ◽  
pp. 469-478 ◽  
Author(s):  
R. A. Heacock ◽  
O. Hutzinger
Keyword(s):  
Sulfur Trioxide ◽  
Chlorosulfonic Acid ◽  
Chromatographic Behavior ◽  
Ultraviolet Spectroscopy ◽  
Solvent Systems

The four isomeric potassium skatolyl sulfates, with the sulfate residue attached to the 4-, 5-, 6-, and 7-positions in the benzene moiety of the skatole molecule, have been synthesized. The four isomers were prepared by the sulfation of the corresponding hydroxyskatoles with either (a) the pyridine – sulfur trioxide complex in pyridine or (b) chlorosulfonic acid in pyridine. The ultraviolet spectroscopy of this group of compounds is discussed together with their paper chromatographic behavior in several different solvent systems.

THE CHEMISTRY OF THE "AMINOCHROMES": PART IV. SOME NEW AMINOCHROMES AND THEIR DERIVATIVES

1960 ◽  
Vol 38 (4) ◽  
pp. 516-527 ◽  
Author(s):  
R. A. Heacock ◽  
B. D. Scott
Keyword(s):  
Acetic Anhydride ◽  
Absorption Spectra ◽  
Methyl Ether ◽  
Ethyl Ether ◽  
Crystalline Form ◽  
Chromatographic Behavior ◽  
Visible Absorption

N-Ethylnoradrenochrome, N-isopropylnoradrenochrome, adrenochrome methyl ether, adrenochrome ethyl ether, and their 2-iodo derivatives have been prepared in crystalline form. The action of acetic anhydride in pyridine on these aminochromes has been studied; acetylated rearrangement products were obtained in each case. N-Ethylnoradrenochrome monosemicarbazone, N-ethylnoradrenolutin, 5,6-diacetoxy-N-ethyl-2-iodoindole, and 5,6-diacetoxy-2-iodo-N-isopropylindole have been prepared. The ultraviolet and visible absorption spectra of the aminochromes described above and several 5,6-diacetoxy- and 3,5,6-triacetoxy-N-alkylindoles have been measured and the paper chromatographic behavior of the unhalogenated aminochromes studied.

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.

Hydrogen-Bonded Solvent Systems

1969 ◽  
Vol 67 (1_3) ◽  
pp. 168-168
Author(s):  
H. G. Hertz
Keyword(s):  
Solvent Systems ◽  
Hydrogen Bonded
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