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

التفاصيل البيبلوغرافية
العنوان: General screening and optimization strategy for fast chiral separations in modern supercritical fluid chromatography
المؤلفون: Michal Douša, Lucie Nováková
المصدر: Analytica Chimica Acta. 950:199-210
بيانات النشر: Elsevier BV, 2017.
سنة النشر: 2017
مصطلحات موضوعية: Diethylamine, Tris, Chromatography, 010405 organic chemistry, Chemistry, 010401 analytical chemistry, 01 natural sciences, Biochemistry, 0104 chemical sciences, Analytical Chemistry, chemistry.chemical_compound, Ammonium formate, Supercritical fluid chromatography, Environmental Chemistry, Methanol, Cellulose, Acetonitrile, Ammonium acetate, Spectroscopy
الوصف: 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: CO 2 /methanol and CO 2 /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.
تدمد: 0003-2670
DOI: 10.1016/j.aca.2016.11.002
URL الوصول: https://explore.openaire.eu/search/publication?articleId=doi_dedup___::ffafa51b5779adecc5d36d38f3e77f8a
https://doi.org/10.1016/j.aca.2016.11.002
Rights: CLOSED
رقم الانضمام: edsair.doi.dedup.....ffafa51b5779adecc5d36d38f3e77f8a
قاعدة البيانات: OpenAIRE
الوصف
تدمد:00032670
DOI:10.1016/j.aca.2016.11.002