In this report the synthesis and characterization of chiral stationary phase of cellulose tris(3,5 dimethylphenylcarbamate) coated zirconia(CDMPC ZrO 2 CSP) was described. Direct optical resolutions of acidic racemate...In this report the synthesis and characterization of chiral stationary phase of cellulose tris(3,5 dimethylphenylcarbamate) coated zirconia(CDMPC ZrO 2 CSP) was described. Direct optical resolutions of acidic racemate naproxen and its derivatives on the phase were investigated. Surface property of zirconia affects the chiral separation of naproxen greatly. Naproxen could not be eluted from the column unless an acidic modifier was present in the mobile phase. However, good chiral resolutions were obtained for its ester derivatives. The influences of loading amount of stationary phase, molecular structure of compounds, type of alcohols as the modifier and their concentration in mobile phase on chiral resolution were studied. The chiral recognition mechanism of the chiral stationary phase was discussed.展开更多
A novel chiral stationary phase(CSP) for HPLC was prepared by synthesizing 3,5-dinitrobenzoyl-(S)-1,2,3,4-tetrahydro-3-isoquinolinecarboxylic acid as chiral selector and bonding it with 3-aminopropylsilane modified si...A novel chiral stationary phase(CSP) for HPLC was prepared by synthesizing 3,5-dinitrobenzoyl-(S)-1,2,3,4-tetrahydro-3-isoquinolinecarboxylic acid as chiral selector and bonding it with 3-aminopropylsilane modified silica.The resolutions of 8 enantiomers of binaphthol and its derivatives were achieved by using hexane-ethanol-acetic acid(98∶2∶0.5,volume ratio) as mobile phase with a column temperature 30 ℃ and detected at ultraviolet 254 nm.The effects of acetic acid and alcohol organic modifiers on retention and resolutions of the analytes were examined.The enantioselectivities α of the analytes on CSP could be improved by adding acetic acid to mobile phase due to masking effect of H^+ on the residing silanol and amino group.展开更多
DMA-LiCl-cellulose is coated on 3-aminopropyl silica gel as chiral stationary phases for high performance liquid chromatography(HPLC),and its chiral column(250 mm×2.0mm,i.d.)was prepared under the pressure of 40 ...DMA-LiCl-cellulose is coated on 3-aminopropyl silica gel as chiral stationary phases for high performance liquid chromatography(HPLC),and its chiral column(250 mm×2.0mm,i.d.)was prepared under the pressure of 40 MPa.In the normal phase of high performance liquid chromatography,21 chiral compounds,including alcohols,acids,amines,amino acids and drugs,were resolved on this column,13 kinds of chiral compounds have been separated.The results indicate that the chiral stationary phase possesses a good chiral separation ability.展开更多
文摘In this report the synthesis and characterization of chiral stationary phase of cellulose tris(3,5 dimethylphenylcarbamate) coated zirconia(CDMPC ZrO 2 CSP) was described. Direct optical resolutions of acidic racemate naproxen and its derivatives on the phase were investigated. Surface property of zirconia affects the chiral separation of naproxen greatly. Naproxen could not be eluted from the column unless an acidic modifier was present in the mobile phase. However, good chiral resolutions were obtained for its ester derivatives. The influences of loading amount of stationary phase, molecular structure of compounds, type of alcohols as the modifier and their concentration in mobile phase on chiral resolution were studied. The chiral recognition mechanism of the chiral stationary phase was discussed.
文摘A novel chiral stationary phase(CSP) for HPLC was prepared by synthesizing 3,5-dinitrobenzoyl-(S)-1,2,3,4-tetrahydro-3-isoquinolinecarboxylic acid as chiral selector and bonding it with 3-aminopropylsilane modified silica.The resolutions of 8 enantiomers of binaphthol and its derivatives were achieved by using hexane-ethanol-acetic acid(98∶2∶0.5,volume ratio) as mobile phase with a column temperature 30 ℃ and detected at ultraviolet 254 nm.The effects of acetic acid and alcohol organic modifiers on retention and resolutions of the analytes were examined.The enantioselectivities α of the analytes on CSP could be improved by adding acetic acid to mobile phase due to masking effect of H^+ on the residing silanol and amino group.
文摘DMA-LiCl-cellulose is coated on 3-aminopropyl silica gel as chiral stationary phases for high performance liquid chromatography(HPLC),and its chiral column(250 mm×2.0mm,i.d.)was prepared under the pressure of 40 MPa.In the normal phase of high performance liquid chromatography,21 chiral compounds,including alcohols,acids,amines,amino acids and drugs,were resolved on this column,13 kinds of chiral compounds have been separated.The results indicate that the chiral stationary phase possesses a good chiral separation ability.
