RESUMO
The physico-chemical properties of trans-5-chloro-2-methyl-2,3,3a,12b-tetrahydro-1H- dibenz[2,3:6,7]oxepino[4,5-c]pyrrolidine maleate (Org 5222), a new potential antipsychotic compound, were studied by interpretation of its spectra (UV,IR,NMR,mass), X-ray analysis, thermal properties, solubilities and partition coefficient. Analytical methods such as GLC and TLC were developed for use in stability tests. Crystalline Org 5222 was shown to be stable with respect to heat. Only excessive exposure to light was shown to induce degradation of crystalline Org 5222. In solutions of pH 1, 4 and 7 only slight degradation was observed at high temperature or after exposure to light.
Assuntos
Antipsicóticos/análise , Dibenzoxepinas/análise , Varredura Diferencial de Calorimetria , Fenômenos Químicos , Química , Físico-Química , Cromatografia em Camada Fina , Dibenzocicloeptenos , Estabilidade de Medicamentos , Compostos Heterocíclicos de 4 ou mais Anéis , Espectroscopia de Ressonância Magnética , Espectrometria de Massas , Solubilidade , Espectrofotometria Infravermelho , Espectrofotometria Ultravioleta , Temperatura , Difração de Raios XRESUMO
The 1H- and 1H-1H correlation (COSY) NMR spectra of human, porcine and bovine insulin have been recorded. The 1.1-1.5 ppm regions of these spectra show the methyl signals of the alanine and threonine residues. The number of alanines and threonines differs for the three insulins and thus allows an easy discrimination with NMR.
Assuntos
Insulina/análise , Animais , Bovinos , Humanos , Espectroscopia de Ressonância Magnética , Especificidade da Espécie , SuínosRESUMO
The regular occurrence of a peak due to an unidentified substance (X) in the gas chromatographic traces obtained from phenolic extracts of urine from human pregnant and non-pregnant females has been reported. The biphasic excretion of X with maxima in the luteal phase of the ovulatory cycle and relatively high levels in the first trimester of pregnancy were noteworthy and suggested that the substance may have a biological significance. Close similarities between the excretory pattern, the chemical and chromatographic properties of X and of those of the known phenolic steroids suggested initially that this compound was steroidal in nature. The same, or a similar, substance seems to be excreted in the vervet monkey (Cercopithecus aethiops pygerythrus). We now report the excretory pattern of X in more detail, the isolation of the pure compound from pooled pregnancy urine and the chemical structure. The structure determined by mass spectrometry, IR spectroscopy and NMR spectrometry is: trans-(+/-)-3,4-bis[(3-hydroxyphenyl)methyl]dihydro-2-(3H)-furanone (HPMF) and was confirmed by synthesis.
