Identification of retinolisomers by high-performance liquid chromatography not unequivocal up to now.

Former publications dealing with high-performance liquid chromatography (HPLC) of retinol provide inconsistent results and lack evidence for the identification of isomers. For clarification of the problems in this field, the isomeric structure of the major retinol isomers in crystallized form was proven by 1H-NMR, UV absorption spectroscopy and by X-ray analysis. These identified isomeric forms of retinol were separated by HPLC with different eluent mixtures and the chromatograms compared in detail with previously published data. A conclusive assignment for HPLC separation of retinol isomers is given.

[1H-NMR spectroscopic study of cysteamine eyedrops]. / 1H-NMR-spektroskopische Untersuchung von Cysteamin-Augentropfen.

BACKGROUND: The efficiency of cysteamine eye drops in the treatment of cystinosis has been demonstrated in several studies: Corneal cystine crystals can be removed by topical cysteamine. Cysteamie 0.5% eye drops were superior to a 0.1% solution. It is not clear how fast cysteamine is oxidized to cystamine under the influence of atmospheric oxygen. MATERIAL AND METHODS: Samples of a new bottled cysteamine 0.5% solution were analysed 1H-NMR-spectroscopically over a period of several weeks (AM 400/WB-NMR-instrument, Bruker/Karlsruhe; 400.15 MHz). Samples bottled in an argon atmosphere were compared to samples bottled without inert gas. Definite samples were opened four times a day (A). The remainder of the samples was stored closed (B). RESULTS: In sample A a 1:1 weight ratio between cysteamine and cystamine was reached after 38 days. In samples B cysteamine was not oxidized to cystamine. The initial amount of cystamine was something lower in samples with argon, but argon could not prevent the decrease of the cysteamine concentration in sample A. CONCLUSIONS: The preparation of cysteamine solution in an argon atmosphere is useful. One bottle can be used for about one week, if less than 10% of the oxidation product cystamine is accepted.

Lung surfactant phospholipids associate with polymerizing fibrin: loss of surface activity.

Intraalveolar fibrin formation is a hallmark of many acute and chronic lung inflammatory processes. We investigated the influence of fibrin polymerization on biochemical and biophysical properties of a calf lung surfactant extract (CLSE) used for therapy of neonatal distress syndrome. Thrombin-induced coagulation of human fibrinogen (range, 0.04 to 4 mg/ml) in the presence of CLSE (2 mg/ml phospholipids) resulted in progressive loss of surface tension-lowering properties and adsorption facilities of this surfactant preparation; the CLSE-inhibitory capacity of desAABB-fibrin surpassed that of fibrinogen by more than two orders of magnitude. In parallel with the loss of surface activity, association of the predominant surfactant phospholipid dipalmitoylphosphatidylcholine (DPPC) (14C-labeled, admixed to 2 mg/ml CLSE) with polymerizing desAABB-fibrin occurred. A volume of 0.3 mg/ml insoluble fibrin effected a approximately 50% loss, and 0.6 mg/ml a > 90% loss, of DPPC from the aqueous phase. Dioleoylphosphatidylcholine, dipalmitoylphosphatidic acid, stearic acid, palmitic acid, and arachidonic acid, admixed to CLSE as labeled compounds, as well as total CLSE phospholipids were retained in polymerizing desAABB-fibrin with dose-effect curves superimposable to that of DPPC; no fibrin association was noted for 14C-glycerol-3-phosphate. Polymerizing desAA-fibrin, generated by incubation of CLSE-fibrinogen mixtures with arvin, captured DPPC and resulted in loss of surface properties at even lower concentrations, compared with desAABB-fibrin. In contrast, CLSE incubation with preformed desAABB- and desAA-fibrin polymers did not cause substantial phospholipid coupling with the clot material or loss of surface properties. Microtiter plate-immobilized fibrinogen and desAABB- and desAA-fibrinomonomers did not bind CLSE phospholipids enriched with 14C-DPPC.(ABSTRACT TRUNCATED AT 250 WORDS)

Paraffin oil pneumonia. Analysis of saturated hydrocarbons in different human tissue.

Temperature-programmed gas chromatographic analysis on columns packed with Apiezon L as stationary phase is shown to be the best method for the qualitative and quantitative analysis of simple and complex hydrocarbon mixtures when compared with all the other applicable techniques (thin-layer chromatography, column chromatography, ultraviolet spectroscopy, infrared spectroscopy, nuclear magnetic resonance spectroscopy, mass spectrometry) described in this paper. Using the method in a patient with mineral oil pneumonia it could be demonstrated that he expectorated a maximum of 79.5 mg liquid paraffin daily and also transported equally complex saturated hydrocarbons in a concentration of 1.3 mg% in plasma and of 1.6 mg% in the cellular blood components. In an additional experiment the direct determination of liquid paraffin resorbed from the gastrointestinal tract was possible in a patient with a left chyle fistula in the neck. After a dose of 50 g liquid paraffin administered as a laxative, 246 ml chyle was collected within the following 14 h which yielded a total of 4.5 mg liquid paraffin. Its composition was identical with the administered laxative. Assuming a daily lymph volume of 1.51, the resorbed amount would correspond to a resorption rate of 0.5 (see article) liquid paraffin. The importance of these results as well as the diagnostic consequences arising from the described analytical technique are discussed in detail.