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超临界流体色谱法手性分离反式氧化苯乙烯保留因子的密度依赖性

Density dependence of retention factors of trans-stilbene oxide for chiral separation by supercritical fluid chromatography.

作者信息

Funazukuri Toshitaka, Ono Yuna, Sakabe Junichi, Kong Chang Yi

机构信息

Department of Applied Chemistry, Chuo University, 1-13-27 Kasuga, Bunkyo-ku, Tokyo, Japan.

Department of Applied Chemistry, Chuo University, 1-13-27 Kasuga, Bunkyo-ku, Tokyo, Japan.

出版信息

J Chromatogr A. 2017 Dec 8;1527:91-96. doi: 10.1016/j.chroma.2017.10.029. Epub 2017 Oct 28.

Abstract

Retention factors for two enantiomers of trans-stilbene oxide, k and k, were measured with a chiral AD-H column using two syringe pumps to feed CO and methanol as a co-solvent at various temperatures, pressures and co-solvent mole fractions to determine the effects of these operating conditions on the retention factors. The retention factors k and k are for the (R,R)- and (S,S)-forms, respectively. When the isothermal compressibilities of a mixture of CO and MeOH were lower than 0.01, far from the critical locus of the CO and methanol mixture, both retention factors were well expressed with the solvent density and temperature with an average absolute relative deviation of 1-2%. In the vicinity of the critical locus, however, where the isothermal compressibilities were much larger than 0.01, the relationship between retention factor and density was complicated. Both retention factors were proportional to the isothermal compressibility, irrespective of methanol mole fraction at each temperature.

摘要

使用手性AD - H柱,通过两个注射泵在不同温度、压力和共溶剂摩尔分数下输送一氧化碳(CO)和甲醇作为共溶剂,测定反式氧化茋两种对映体的保留因子k₁和k₂,以确定这些操作条件对保留因子的影响。保留因子k₁和k₂分别对应(R,R)-和(S,S)-形式。当CO和甲醇混合物的等温压缩率低于0.01,远离CO和甲醇混合物的临界轨迹时,两个保留因子都能很好地用溶剂密度和温度表示,平均绝对相对偏差为1 - 2%。然而,在临界轨迹附近,等温压缩率远大于0.01时,保留因子与密度之间的关系变得复杂。在每个温度下,无论甲醇摩尔分数如何,两个保留因子都与等温压缩率成正比。

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