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Biomedical subjects

G Balogh

Publications and source records attributed to G Balogh.

At least 55 records · Page 3Linked to original sources

[Analysis of steroids. Part 40. Isolation and identification of unusual impurities in ethynodiol diacetate].

In the course of the estimation of the impurity profile of ethynodiol diacetate, in addition to common impurities such as norethisterone acetate, ethynodiol-3-acetate and alpha-ethynodiol diacetate, two unknown impurities were detected by analytical reversed phase HPLC (C-18 silica and 80% aq. methanol as the eluent) and isolated by normal phase preparative HPLC (silica and 98:2 mixture of hexane and 2-propanol as the eluent). The 1H- and 13C-NMR spectra of the isolated impurities revealed that their structures could be characterized as the E and Z isomers of an analogue of EDDA containing "trimerised acetyl" group at the 17-hydroxy group (structures 4 and 4a). These structures were in good agreement with the extended UV spectra of the impurities and the mass spectra with the m/z 438 peak which can be derived from 4 and 4a by the loss of ketene.

Chromatography, High Pressure Liquid↗

[Analysis of steroids. Part 42. By-products of the ethynylation of 17-ketosteroids (isolation, identification and determination)].

The therapeutically very important 17 alpha-ethynyl steroids are prepared from 17-keto steroids by means of addition of acetylene. Two important side reactions of this procedure are known: the formation of the isomeric beta-ethynyl derivative and the formation of a dimeric product with acetylene bridge. The aim of this paper is to approach this problem from the point of view of impurity profiling of 17 alpha-ethynyl steroids (norethisterone, ethisterone, norgestrel and delta 9(11)-ethisterone) i.e. isolation, identification and quantification of the above mentioned by-products as impurities in the bulk drugs. Capillary gas chromatography is an ideal tool for the separation and quantitative determination of the beta-ethynyl derivatives (20 m long fused silica capillary, I.D 0.2 mm; stationary phase Ultra-2: 5% phenylmethyl silicon gum phase with a film thickness of 0.33 mu; column temperature 240-250 degrees C). The dimeric impurity cannot be determined directly by gas chromatography as it decomposes in the flash heater to the 17 alpha-ethynyl and the 17-keto derivatives. For this reason reversed-phase HPLC was preferred for their separation and quantitation; (column: 250 x 4 mm LiChrosorb RP-18, 10 microns; eluent methanol-water 7:3; UV detector 240 nm). The HPLC method is suitable for the separation and determination of the beta-ethynyl impurities, too. The chemical shifts of the protons and carbon atoms in the vicinity of C-17 in the 1H and 13C NMR spectra of the epimeric 17-ethynyl steroids greatly depend on the configuration of the ethynyl group and for this reason they (especially that of the C-18 are eminently suitable for the characterization of the isomers.(ABSTRACT TRUNCATED AT 250 WORDS)

17-Ketosteroids↗

Detection of different functional states of the cellular nucleus with a new trichrome staining technique.

The new trichrome stain ASTRIN, prepared from alcian blue, safranine, thionine, and resorcin, stains the cell nuclei red or blue, depending on their functional state. Activation of salivary gland cells with pilocarpin, or of liver cell with prednisolone, equally resulted in a quantitative increase of cells with active (blue) nuclei. Changes in nuclear staining after digestion with trypsin, pronase, or ribonuclease, and after extraction of cellular DNA and RNA with perchloric acid, unequivocally suggest that alteration of the protein-DNA ratio, i.e. the hetero- or euchromatic state of nuclear chromatin, is responsible for the disparity of the nuclear staining reaction with ASTRIN. The new trichrome stain seems to be suitable for routine cytodiagnostic use.

Animals↗

ASTRIN - a new trichrome staining technique.

The new trichrome stain ASTRIN, composed of alcian blue, safranine, thionine and resorcin, differentiates myocytes from fibrocytes, mature from immature cartilagineous elements, heterochromatic from euchromatic state of nuclear chromatin, and detects neurosecretions. The great differential staining potential of ASTRIN is in all probability due to the dissimilar diffusion rates of its components, for no new dye molecule arises from the combination, as shown by spectrophotometric and thin-layer chromatographic analysis.

Alcian Blue↗

A critical re-evaluation of the anisotropic index used in polarization microscopy: a study on epiphyseal cartilage.

Topo-optical reactions specific for collagen and glycosaminoglycans were performed on epiphyseal cartilage plates which differed in age, in chemical composition, and in structure. Retardation values were measured with the polarization microscope and anisotropic index values were calculated after each reaction. It was found that the anisotropic index proposed earlier for quantitative evaluation of topo-optical reactions did not refer either to the submicroscopic orientation pattern or to the quantity of cartilage matrix components. It is suggested that retardation values of induced birefringence may be only used to characterize the spatial orientation of these components in the cartilage matrix.

Aging↗