DILUTED VERSUS UNDILUTED CYCLODEXTRIN DERIVATIVES IN CAPILLARY GAS-CHROMATOGRAPHY AND THE EFFECT OF LINEAR CARRIER GAS VELOCITY, COLUMN TEMPERATURE, AND LENGTH ON ENANTIOMER SEPARATION

被引:46
作者
HARDT, I [1 ]
KONIG, WA [1 ]
机构
[1] UNIV HAMBURG,INST ORGAN CHEM,W-2000 HAMBURG 13,GERMANY
关键词
ENANTIOMERS; GAS CHROMATOGRAPHY; CYCLODEXTRIN DERIVATIVES; TEMPERATURE DEPENDENCE; CAPILLARY COLUMNS; SELECTIVITY;
D O I
10.1002/mcs.1220050105
中图分类号
O65 [分析化学];
学科分类号
070302 ; 081704 ;
摘要
The effect of dilution of the chiral stationary phase octakis(3-O-butyryl-2,6-di-O-pentyl)-gamma-cyclodextrin in the achiral polysiloxane OV-1701 on the separation factor was investigated over a wide concentration range. The loss in enantioselectivity was only negligible down to a dilution of 50 % (w/w), since the separation factor vs. concentration curves levels off at higher concentrations. Because of the strong temperature dependence of the separation factors, the properties of short columns (10 m and 4.5 m) were evaluated. These short columns, which allow operation at low temperatures and lead to enhanced separation factors were found to be appropriate for the separations of simple mixtures, because the gain in selectivity exceeded the loss in separation efficiency. For complex mixtures, the higher efficiencies of columns of at least 25 m in length were still necessary. A plot of In alpha vs. 1/T did not yield straight lines, but showed a significant curvature, leading to considerable relative errors if thermodynamic data were derived from these plots.
引用
收藏
页码:35 / 40
页数:6
相关论文
共 16 条
  • [1] A STATIC COATING PROCEDURE FOR GLASS CAPILLARY COLUMNS
    BOUCHE, J
    VERZELE, M
    [J]. JOURNAL OF GAS CHROMATOGRAPHY, 1968, 6 (10): : 501 - &
  • [2] GROB K, 1990, HRC-J HIGH RES CHROM, V13, P433
  • [3] Grob K., 1986, MAKING MANIPULATING
  • [4] THEORETICAL APPROACH TO THE GAS-CHROMATOGRAPHIC SEPARATION OF ENANTIOMERS ON DISSOLVED CYCLODEXTRIN DERIVATIVES
    JUNG, M
    SCHMALZING, D
    SCHURIG, V
    [J]. JOURNAL OF CHROMATOGRAPHY, 1991, 552 (1-2): : 43 - 57
  • [5] KEIM W, 1991, HRC-J HIGH RES CHROM, V14, P507
  • [6] Konig W. A., 1992, GAS CHROMATOGRAPHIC
  • [7] APPLICATION OF ENANTIOSELECTIVE CAPILLARY GAS-CHROMATOGRAPHY TO THE ANALYSIS OF CHIRAL PHARMACEUTICALS
    KONIG, WA
    ERNST, K
    [J]. JOURNAL OF CHROMATOGRAPHY, 1983, 280 (01): : 135 - 141
  • [8] Konig WA, 1989, J HIGH RES CHROMATOG, V12, P732, DOI DOI 10.1002/JHRC.1240121108
  • [9] Konig WA, 1991, J HIGH RES CHROMATOG, V14, P694
  • [10] KONIG WA, 1990, KONTAKTE DARMSTADT, V2, P3