General screening and optimization strategy for fast chiral separations in modern supercritical fluid chromatography

Result code in IS VaVaI

<a href="https://www.isvavai.cz/riv?ss=detail&h=RIV%2F00216208%3A11160%2F17%3A10365394" target="_blank" >RIV/00216208:11160/17:10365394 - isvavai.cz</a>

Result on the web

<a href="http://www.sciencedirect.com/science/article/pii/S0003267016312879" target="_blank" >http://www.sciencedirect.com/science/article/pii/S0003267016312879</a>

DOI - Digital Object Identifier

<a href="http://dx.doi.org/10.1016/j.aca.2016.11.002" target="_blank" >10.1016/j.aca.2016.11.002</a>

Result language

angličtina

Original language name

General screening and optimization strategy for fast chiral separations in modern supercritical fluid chromatography

Original language description

High throughput general chiral screening method using supercritical fluid chromatography was developed. This method takes an advantage of very fast gradient screening (3 min + 1 min isocratic hold) and generic enantioselectivity of the combined additive formed by 0.1% trifluoroacetic (TFA) acid and 0.1% diethylamine (DEA). The TFA/DEA combined additive was systematically added to organic modifiers methanol and isopropanol. Among five tested polysaccharide-based chiral stationary phases, amylose tris(3,5-dimethylphenylcarbamate) and cellulose tris(3,5-dimethylphenylcarbamate) provided the best enantioseparation success rate. Therefore, the proposed initial first-line screening includes four experiments using these two stationary phases and the above mentioned two combinations: CO2/methanol and CO2/isopropanol + the combined additive. If these stationary phases fail in the screening step, cellulose tris(3-chloro-4-methylphenylcarbamate) and cellulose tris(3,5-dichlorophenylcarbamate) can be proposed for the screening in the second line. For further optimization in case of insufficient resolution obtained in the screening phase fine tuning of temperature, BPR pressure and gradient slope was tested with unsuccessful results. An improvement of enantioselectivity was obtained only when gradient elution was replaced by isocratic elution with substantially lower amount of organic modifier, when changing the concentration of the additive or when using combined organic modifier, such as methanol/acetonitrile (1:1). Finally, to enable the MS compatibility, also volatile additives including ammonium formate and ammonium acetate were tested. The results were more encouraging than expected. Volatile buffers thus make an interesting option in chiral SFC screening methods, however, at the cost of somewhat lower enantioselectivity.

Czech name

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Czech description

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Type

J_imp - Article in a specialist periodical, which is included in the Web of Science database

CEP classification

—

OECD FORD branch

30104 - Pharmacology and pharmacy

Project

—

Continuities

I - Institucionalni podpora na dlouhodoby koncepcni rozvoj vyzkumne organizace

Publication year

2017

Confidentiality

S - Úplné a pravdivé údaje o projektu nepodléhají ochraně podle zvláštních právních předpisů

Name of the periodical

Analytica Chimica Acta

ISSN

0003-2670

e-ISSN

—

Volume of the periodical

950

Issue of the periodical within the volume

January

Country of publishing house

NL - THE KINGDOM OF THE NETHERLANDS

Number of pages

12

Pages from-to

199-210

UT code for WoS article

000390629500023

EID of the result in the Scopus database

2-s2.0-84999723821