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Titolo:
Chiral separations of metoprolol and some analogs with carbon dioxide on Chiralcel OD and Chiralpak AD stationary phases. Use of chemometrics
Autore:
Svensson, S; Karlsson, A; Gyllenhaal, O; Vessman, J;
Indirizzi:
AstraZeneca R&D Molndal, S-43183 Molndal, Sweden AstraZeneca R&D Molndal Molndal Sweden S-43183 , S-43183 Molndal, Sweden
Titolo Testata:
CHROMATOGRAPHIA
fascicolo: 5-6, volume: 51, anno: 2000,
pagine: 283 - 293
SICI:
0009-5893(200003)51:5-6<283:CSOMAS>2.0.ZU;2-B
Fonte:
ISI
Lingua:
ENG
Soggetto:
SUPERCRITICAL-FLUID-CHROMATOGRAPHY; BETA-BLOCKERS; ENANTIOSELECTIVE SEPARATION; ENANTIOMERIC SEPARATION; CHYROSINE-A; COLUMN; TEMPERATURE; RESOLUTION; LIQUID; HPLC;
Keywords:
supercritical-fluid chromatography; enantiomer separation; amino alcohols; statistical experimental design;
Tipo documento:
Article
Natura:
Periodico
Settore Disciplinare:
Life Sciences
Physical, Chemical & Earth Sciences
Citazioni:
30
Recensione:
Indirizzi per estratti:
Indirizzo: Karlsson, A AstraZeneca R&D Molndal, S-43183 Molndal, Sweden AstraZeneca R&D Molndal Molndal Sweden S-43183 lndal, Sweden
Citazione:
S. Svensson et al., "Chiral separations of metoprolol and some analogs with carbon dioxide on Chiralcel OD and Chiralpak AD stationary phases. Use of chemometrics", CHROMATOGR, 51(5-6), 2000, pp. 283-293

Abstract

The influence of methanol concentration, column temperature, and column back-pressure on the enantioselectivity of the separation of eighteen amino alcohols in supercritical-fluid chromatography has been investigated by use of statistical experimental design. The enantioselective retention of the amino alcohols was studied using Chiralcel OD and Chiralpak AD as the chiralstationary phases and the experimental responses obtained - retention factors (k) and selectivity factors (alpha) - were evaluated by use of the partial least squares algorithm. The performance of the columns was compared and the enantioselectivity of the Chiralcel OD column was found to be superior. Almost all the racemic amino alcohols tested were separated and separation factors as high as 4.5 were obtained by use of the Chiralcel OD column. Experimental results from a factorial design with three centerpoints resulted in a statistical model based on linear terms only. The first-eluted enantiomers, which, when identified, were found to be the Ii forms, had similar retention times, whereas the retention times of the S forms were more varied. The column temperature had a greater effect on enantioselectivity thanmethanol content. Changes in the system back-pressure had no significant influence on enantioselectivity. The results obtained from the factorial design were used to predict k and a. Differences between predicted and experimental data were less than 10 %. The effect on enantioselectivity of protolytic mobile phase additives, e.g. dimethyloctylamine, acetic acid, and trifluoroacetic acid, and of mobile-phase flow-rate, were also studied, as was the effect of solute structure. The position of substituents on the aromatic ring, type of alkyl group attached to the nitrogen atom, and the number of methylene groups between the stereogenic center and the nitrogen atom all affected enantioselectivity. The chromatographic system developed could be used to determine enantiomeric purity even if the chiral impurity eluted after the main peak.

ASDD Area Sistemi Dipartimentali e Documentali, Università di Bologna, Catalogo delle riviste ed altri periodici
Documento generato il 20/09/20 alle ore 10:21:50