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超临界流体色谱( SFC)分离具有速度快、分离效率高、溶剂消耗少等优点,近年来在手性化合物的分离分析中得到诸多应用。本文对比研究了涂覆型多糖手性色谱柱在 SFC和高效液相色谱( HPLC)上拆分24种手性化合物的差异。通过比较这些化合物在色谱柱上的保留时间和选择因子等发现多数化合物在 SFC 上的分离效率要高于其在 HPLC上的分离效率,但 HPLC对轴手性化合物的分离效率要优于 SFC。SFC 和 HPLC 的分离表现出一定的互补性,随着苯环侧链烷基的碳数增加,化合物在 SFC上的保留逐渐增强,而在 HPLC的保留却逐渐减弱。叶菌唑在使用 SFC和 HPLC分析时出现了洗脱顺序反转的现象。这些结果为 SFC手性拆分提供了参考。

Supercritical fluid chromatographic( SFC)technique has been widely applied in the analysis,determinations and chromatographic preparations of chiral compounds in past decades due to some advantages such as fast speed,high efficiency and low consumption of organic sol-vents. Herein,24 kinds of chiral compounds(H1-H24)have been resolved on four polysaccha-ride-coated chiral stationary phases( CSPs)by SFC and high performance liquid chromatogra-phy( HPLC ),separately. Taking into account their retention times and selection factors of these compounds,SFC separation showed a better efficiency than HPLC for most of the com-pounds,except for some axis-chiral compounds. Some complementarity between SFC and HPLC separations was observed. For H15-H17,their retentions in SFC separations showed a strengthening trend with increasing carbon numbers of side alkyl chain,whereas a reverse tend-ency in HPLC separation was displayed. Most interestingly,an elution order reversal of metcon-azole enantiomers was found in this work. In brief,these results would provide some valuable references for the development of SFC separation methods in the future.

参考文献

[1] Payagala, T.;Wanigasekara, E.;Armstrong, D.W..Synthesis and chromatographic evaluation of new polymeric chiral stationary phases based on three (1S,2S)-(-)-1,2-diphenylethylenediamine derivatives in HPLC and SFC[J].Analytical and bioanalytical chemistry,20117(7):2445-2461.
[2] Lin, C.;Liu, W.;Fan, J.;Wang, Y.;Zheng, S.;Lin, R.;Zhang, H.;Zhang, W..Synthesis of a novel cyclodextrin-derived chiral stationary phase with multiple urea linkages and enantioseparation toward chiral osmabenzene complex[J].Journal of chromatography, A: Including electrophoresis and other separation methods,2013:68-74.
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