Determination of panaxadiol and panaxatriol in ginseng and its preparations by capillary supercritical fluid chromatography (SFC).

Capillary supercritical fluid chromatographic (SFC) method has been developed for the determination of panaxadiol and panaxatriol in ginseng and its preparations. 0.1 g ginseng or an appropriate amount of its preparations was hydrolysed by 15% H2SO4 in an ethanol:water (1:1 v/v) solution for 4 h followed by 15% NaOH for 0.5 h. The mixture was extracted by cyclohexane. The cyclohexane extracts were purified by a partition column and concentrated by an adsorption column and then analysed by SFC. Methyltestosterone was used as the internal standard.     

New catalytic method for the synthesis of vitamins K

A new catalytic method for the synthesis of vitamins of the K family is suggested. In this method 2-methyl-1-naphthol is oxidized by dioxygen in the presence of Mo-V-P heteropoly acids or their salts in a two-phase system (organic solvent + water) to 2-methyl-1,4-naphthoquinone or vitamin K3, which is the precursor of all K family vitamins.     

Membrane filtration studies of aquatic humic substances and their metal species: a concise overview. Part 2. Evaluation of conditional stability constants by using ultrafiltration

The assessment of conditional stability constants of aquatic humic substance (HS) metal complexes is overviewed with special emphasis on the application of ultrafiltration methods. Fundamentals and limitations of stability functions in the case of macromolecular and polydisperse metal-HS species in aquatic environments are critically discussed. The review summarizes the advantages and application of ultrafiltration for metal-HS complexation studies, discusses the comparibility and reliability of stability constants. The potential of ultrafiltration procedures for characterizing the lability of metal-HS species is also stressed.     

Thermodynamic properties of aluminum monooxycarbide Al2OC

It was shown that the published data on the thermodynamic properties of aluminum monooxycarbide Al₂OC (ed) are not consistent with the phase diagram of the Al₂O₃-Al₄C₃ system. A thermodynamic modeling of the equilibrium state of the Al₂O₃-Al₄C₃ system made it possible to obtain new estimates of the standard entropy and enthalpy of formation of aluminum monooxycarbide: S°(298.15 K, cd. Al₂OC) = 45.3 J/(K mol) and Δ_f H°(298.15 K, cd, Al₂OC) = ?625.6 kJ/mol.     

New data on the molecular compounds of stereoisomeric ditertiary glycols of the series 1,4-di-(α-hydroxy-sec-alkyl)-cyclohexanes

Summary 1¹,4¹-Dihydroxy-1¹,4¹-diethyl-1,4-dipropylcyclohexanes, like the previously described 1¹,4¹-dihydroxy-1¹,4¹-dimethyl-1,4-diethylcyclohexanes, give a molecular compound of three molecules of cis- and one molecule of trans-form.     

Über die Cyclisierung von Histidinderivaten

Cyclisierung vonl-Histidin-methylester und Histamin über die (nicht isolierten) N-Phenylthiocarbonyl-derivate (Ia) führt durch intramolekulare Harnstoffbildung zu Derivaten des neuartigen bicyclischen Ringsystems Imidazo(1,5-c)tetrahydrooxopyrimidin (II, III).Dieses ist relativ beständig gegen saure Hydrolyse; Einwirkung von basischen Reagenzien (Alkali und Amine) und von Lithiumaluminiumhydrid führt unter Öffnung des Pyrimidinringes (zwischen 4 und 5) zur Bildung von 4(5)-substituierten Imidazolderivaten, wobei mit Aminen N-Carbonsäure-amide (V bis IX) und mit LAH in der Seitenkette N-methylierte Produkte (X, XI) entstehen.Untersuchungen an offenkettigen Modellsubstanzen mit ähnlicher Struktur (XVI, XVII) führten zu ähnlichen Ergebnissen — Abspaltung von Imidazol und entsprechender Substitution der zweiten Komponente, die in manchen Fällen primär als Isocyanat abgespalten wird. Für diese Reaktionen wird ein möglicher Mechanismus diskutiert.DieR _F-Werte einiger Imidazolderivate wurden bestimmt.     

Flow injection-spectrophotometric determination of cresol compounds in water by reaction withp-aminophenol

A spectrophotometric method has been developed for the simultaneous determination ofo-cresol andm-cresol in water by reaction withp-aminophenol (PAP). Three different methodologies have been assayed; (i) batch analysis, after reaction in an alkaline medium in the presence of dissolved molecular oxygen as oxidizing agent, (ii) a stopped-flow procedure, carried out in the presence of KIO₄ and (iii) a flow injection method based on the same approach. The batch procedure requires 22 min for the full development of colour witho-cresol and 12 min form-cresol. In the stopped-flow mode, using KIO₄ and a reaction time of 12 min, better sensitivity can be obtained for both compounds and limits of detection of 10 g 1^–1 foro-cresol and 30 g 1^–1 form-cresol were found. The flow injection method has a lower sensitivity but permits more than 80 injections per hour. Based on the different maximum absorbance wavelengths obtained for the reaction products of PAP witho-cresol (614 nm) andm-cresol (632 nm), both compounds can be simultaneously determined in water samples and recoveries of 90 to 115% were found in spiked water samples of different types.     

Spectrophotometric determination of clotrimazole in bulk drug and dosage forms

A simple, specific, rapid and sensitive spectrophotometric method has been developed for the assay of clotrimazole, in bulk drug and its pharmaceutical preparations. This method is based on the ion-pair complex reaction of clotrimazole and methyl orange in aqueous methanol, and in the presence of citric acid. The chromogen, being extractable with chloroform, could be measured quantitatively at 422 nm. All variables were studied to optimize the reaction conditions. Regression analysis of beer's plot showed good correlation in a general concentration range of 2-14 mu/ml. The proposed method has been successfully applied for the analysis of the bulk drug and its dosage forms such as powder, vaginal tablets, topical solution and creams. No interference was observed from betamethasone dipropionate (Lotriderm cream) or dexamethasone acetate and azidamphenicol (Baycuten cream) or other common pharmaceutical adjuvants. In addition, this method was also found to be specific for the analysis of clotrimazole in the presence of its hydrolytic products as well as imidazole, as a possible impurity.     

Improvement of the HPLC analysis of anthocyanins in red wines by use of recently developed columns

Comparison of the separation performance of five newly developed pH-stable HPLC columns is described for the analysis of anthocyanins in red wines. Separation of twenty anthocyanins in a single run is described using the most appropriate method.     

Bestimmung des Oxydationszustandes in Vanadiumkomplexen mit Hilfe von V—K-Röntgenabsorptionsspektren

Determination of the Oxydation State in Vanadium Complexes using V—K-Absorption Spectra The compounds resulting from the reaction of oxovanadium(IV) sulfate with 8-quinolinols in air were characterized by magnetic moments and V—K-absorption spectra. 8-quinolinol and its Mannich derivates (“CMAB-oxine”, “CMAP-oxine”) form vanadium(V) complexes. The oxovanadium(IV) compound of 7-methyl-8-quinolinol initially formed is not very stable in solution and tends to oxydation. Only the oxovanadium(IV) complex of 2-methyl-8-quinolinol has a good stability corresponding to that of β-diketone compounds.