RESUMO
The equilibria in deuterium oxide solutions of the diamine, 4,4'-methylenebis(tetrahydro-1,2,4-thiadiazine-1,1-dioxide), were studied using highfield (1)H- and (13)C-NMR with the aid of solutions of tetrahydro-2H-1,2,4-thiadiazine-1,1-dioxide (taurultam), its two N-methyl detivatives and methylene glycol. Comparison of the (1)H-NMR spectrum of taurolidine with the one obtained from a mixture of taurultam and methylene glycol indicated that the same equilibria exists in both these solutions. It was concluded that taurolidine, taurultam and its 4-hydroxymethyl adduct and methylene glycol are the major components present. To facilitate the interpretation of the (13)C-spectra, (13)C-enriched methylene glycol was added to solutions of taurultam. The (13)C-studies confirmed the (1)H-NMR study.
RESUMO
Biogenic amines in the brain of the American cockroach have been identified and quantified by an extraction-derivatisation procedure involving their reaction with ditrifluoromethylbenzoyl chloride (DTFMB) in the aqueous phase followed by extraction into an organic solvent, hydrolysis of phenolic esters and conversion of free hydroxyl groups to trimethylsilyl (TMS) ethers and subsequent analysis by gas chromatography-negative ion chemical ionisation mass spectrometry. The molecular ion of these DTFMB-TMS derivatives carried most of the ion current which made the method highly specific and gave a potential limit of detection below the picogram level. This method establishes unequivocally that the principal amines in cockroach brain are tyramine, p-octopamine, dopamine, 5-hydroxytryptamine and noradrenaline. In contrast to mammalian nervous tissue, the other positional isomers of octopamine, together with the isomeric synephrines, are absent.
Assuntos
Aminas Biogênicas/análise , Química Encefálica , Baratas/metabolismo , Animais , Cromatografia Gasosa-Espectrometria de Massas/métodosRESUMO
The determination of the particle size of Intralipid fat emulsions by the non-perturbing method of photon correlation spectroscopy has been extended to include particle size determination using the Coulter counter and optical microscopy. Although little increase in particle size in 3-litre bags containing total parenteral nutrition mixtures was observed with the methods involving large dilutions, creaming was observed and optical microscopy showed aggregation and some coalescence to have taken place. The problem of re-dispersion upon dilution of aggregated (but not coalesced) fat emulsions makes direct optical observation essential in assessing the stability and safety of such fat emulsion mixtures. The effect of electrolytes (NaCl and CaCl2) on creaming, particle size and electrophoretic mobility showed both minimum stability and minimum zeta potential at 3 X 10(-3) mol dm-3 CaCl2 and at 2.5 X 10(-1) mol dm-3 NaCl. Thus, these maximum levels for electrolytes in total parenteral mixtures are indicated.
Assuntos
Emulsões Gordurosas Intravenosas/análise , Nutrição Parenteral Total , Nutrição Parenteral , Adulto , Cálcio/farmacologia , Química Farmacêutica , Embalagem de Medicamentos , Estabilidade de Medicamentos , Eletrólitos/análise , Eletrólitos/farmacologia , Eletroforese , Humanos , Microquímica , Tamanho da Partícula , Espectrofotometria/instrumentação , Espectrofotometria/métodos , Propriedades de SuperfícieRESUMO
The NMR spectrum of taurolidine in deuterium oxide was compared with spectra obtained from model experiments with amines and formaldehyde. Head-space analysis combined with capillary GC showed that there was less than 0.004% free formaldehyde present in 2% solutions of taurolidine. This value is comparable to the concentration of formaldehyde found when the taurolidine solutions were injected directly onto GC columns.