PubMed · 376039
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H J Waal-Manning, P Bolli. 1979-04-21. Cardioselective beta-blockade and renal function.. https://doi.org/10.1136/bmj.1.6170.1082-a
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The molecular structure of conformational isomorphs given by X-ray diffraction for racemic and enantiomeric atenolol were optimized at the HF/6-31G* level of theory and the infrared spectra of the structure were calculated. These spectra are used to characterize the differences between the various atenolol conformers. The spectra of the (R,S)- and S-atenolol solid forms were recorded and the bands corresponding to the functional groups identified with the aid of the calculated spectra, fitting analysis, temperature effect and H/D isotopic exchange. Particular attention was paid to the stretch vibration modes of the functional groups present in the atenolol.
This paper describes a strategy for the development of chromatographic methods for drug candidates based upon the use of simple MS compatible mobile phases and optimization of the chromatographic selectivity through variations of the stationary phase and mobile phase pH. The strategy employs an automated column selection system and a series of HPLC columns, varying in hydrophobicity and silanol activity, in combination with DryLab software to develop chromatographic methods for the separation of mixtures of bupivacaine and its metabolites; acidic, basic, and neutral compounds; and atenolol, nitrendipine, and their degradation products.
Capillary electrophoresis (CE), using highly-sulfated cyclodextrins as chiral selectors, has been applied to determine the chiral purity of pharmaceutical compounds. A chiral separation strategy, developed earlier for racaemic mixtures, was applied on four basic drugs (propranolol, atenolol, chlorpheniramine and tryptophan methylester). The aim was to develop validated separation methods which allow determination of 0.1% impurity levels of the unwanted enantiomers (distomer) in the presence of 99.9% of the active compound (eutomer). The linearity, quantification limits for the trace enantiomers and the precision of the measurements were determined. In a second part, impurity separations have been simulated in order to evaluate the required resolution when assaying impurities. It is shown that a baseline resolution of 1.5, generally accepted for racaemic mixtures, does not always allow good impurity determinations. Two alternative methods to solve this problem have been proposed.