Analytical and semipreparative high performance liquid chromatography enantio separation of new substituted 1-thiocarbamoyl-3,5-diaryl-4,5-dihydro-(1H)-pyrazoles on polysaccharide-based chiral stationary phases in normal-phase, polar organic and reversed-phase conditions

被引:53
作者
Cirilli, R
Simonelli, A
Ferretti, R
Bolasco, A
Chimenti, P
Secci, D
Maccioni, E
La Torre, F
机构
[1] Ist Super Sanita, Dipartimento Farmaco, I-00161 Rome, Italy
[2] Univ Roma La Sapienza, Dipartimento Studi Chim & Tecnol Sostanze Biol At, I-00185 Rome, Italy
[3] Univ Cagliari, Dipartimento Farmaco Chim Tecnol, I-09124 Cagliari, Italy
关键词
enantioselective HPLC; polysaccharide-based chiral stationary phases; chiralpak IA; semipreparative scale enantioseparation;
D O I
10.1016/j.chroma.2005.10.003
中图分类号
Q5 [生物化学];
学科分类号
071010 ; 081704 ;
摘要
The direct HPLC enantioseparation of five pairs of new chiral pyrazole derivatives on coated cellulose- and amylose-based chiral stationary phases (Chiralpak AD, Chiralcel OJ and Chiralcel OJ-RH) and new immobilised amylose-based Chiralpak IA CSP was performed. Very high enantioselectivity factor (a) values were achieved in polar organic and reversed-phase conditions by using OJ-RH as CSP. Chiralpak IA exhibited an excellent chiral resolving ability in normal-phase mode and it allowed the enantioseparation of analytes investigated with resolution factors (Rs)> 20. Due to its bonded nature, it was successfully employed at analytical and semipreparative scale in combination with normal-phase eluents containing "non-standards" solvents such as acetone. (c) 2005 Elsevier B.V. All rights reserved.
引用
收藏
页码:198 / 203
页数:6
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