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Cellulose tris-(3,5-dimethylphenylcarbamate)-based chiral stationary phase for the enantioseparation of drugs in supercritical fluid chromatography: comparison with HPLC
被引:38
作者:
Kalikova, Kveta
[1
]
Martinkova, Monika
[1
]
Schmid, Martin G.
[2
]
Tesarova, Eva
[1
]
机构:
[1] Charles Univ Prague, Fac Sci, Dept Phys & Macromol Chem, Albertov 2030, Prague 12843, Czech Republic
[2] Karl Franzens Univ Graz, Inst Pharmaceut Sci, Dept Pharmaceut Chem, Graz, Austria
关键词:
cellulose;
chiral stationary phases;
enantioselective separation;
high-performance liquid chromatography;
supercritical fluid chromatography;
RECOGNITION MECHANISMS;
LIQUID-CHROMATOGRAPHY;
CAPILLARY ELECTROCHROMATOGRAPHY;
MOBILE PHASES;
AMYLOSE;
SEPARATION;
INSIGHTS;
PERFORMANCE;
DERIVATIVES;
MODES;
D O I:
10.1002/jssc.201701341
中图分类号:
O65 [分析化学];
学科分类号:
070302 ;
081704 ;
摘要:
A cellulose tris-(3,5-dimethylphenylcarbamate)-based chiral stationary phase was studied as a tool for the enantioselective separation of 21 selected analytes with different pharmaceutical and physicochemical properties. The enantioseparations were performed using supercritical fluid chromatography. The effect of the mobile phase composition was studied. Four different additives (diethylamine, triethylamine, isopropylamine, and trifluoroacetic acid) and isopropylamine combined with trifluoroacetic acid were tested and their influence on enantioseparation was compared. The influence of two different mobile phase co-solvents (methanol and propan-2-ol) combined with all the additives was also evaluated. The best mobile phase compositions for the separation of the majority of enantiomers were CO2/methanol/isopropylamine 80:20:0.1 v/v/v or CO2/propan-2-ol/isopropylamine/trifluoroacetic acid 80:20:0.05:0.05 v/v/v/v. The best results were obtained from the group of basic beta-blockers. A high-performance liquid chromatography separation system composed of the same stationary phase and mobile phase of similar properties prepared as a mixture of hexane/propan-2-ol/additive 80:20:0.1 v/v/v was considered for comparison. Supercritical fluid chromatography was found to yield better results, i.e. better enantioresolution for shorter analysis times than high-performance liquid chromatography. However, examples of enantiomers better resolved under the optimized conditions in high-performance liquid chromatography were also found.
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页码:1471 / 1478
页数:8
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