Enantiomer resolution of D- and L-alpha-amino acid derivatives by supercritical fluid chromatography on novel chiral diamide phases with carbon dioxide.
Enantiomer resolution of D- and L-alpha-amino acid derivatives by supercritical fluid chromatography on novel chiral diamide phases with carbon dioxide.
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通过超临界流体色谱法在新型手性二酰胺相上用二氧化碳拆分 D- 和 L-α-氨基酸衍生物的对映体。
DOI：
10.1016/s0021-9673(00)94281-x
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发表时间：
1989
期刊：
影响因子：
--
通讯作者：
Y. Yamauchi
中科院分区：
文献类型：
--
作者：
A. Dobashi;Y. Dobashi;Tamami Ono;Shoji Hara;Muneo Saito;S. Higashidate;Y. Yamauchi
采用超临界流体色谱（SFC）技术，在新型手性缬氨酸二酰胺相上，以二氧化碳和极性甲醇为改性剂，实现了N-4-硝基苯甲酰基氨基酸异丙酯对映体的快速拆分。在每个固定相中，手性部分通过长的十亚甲基间隔基锚定到硅胶表面。SFC中的对映体选择性与使用2-丙醇-正己烷的液相色谱中的对映体选择性相当。分析所需时间小于5 min，对映体分离度（Rs）范围为10.8-1.25。在使用2-丙醇代替甲醇时，分离得到改善，但伴随着柱效率的降低。对映体拆分剩余的表面硅烷醇的封端效果进行了讨论。
The rapid resolution of racemic N-4-nitrobenzoylamino acid isopropyl esters was accomplished without the loss of enantioselectivity by supercritical fluid chromatography (SFC) on novel chiral valine—diamide phases with carbon dioxide and a polar methanol modifier. In each stationary phase, a chiral moiety was anchored to the silica gel surface by a long decamethylene spacer. The anantioselectivity in SFC was comparable to that in liquid chromatography using 2-propanol-n-hexane. The time required for analysis was less than 5 min, and the range of enantiomer resolution (Rs) was 10.8–1.25. On using 2-propanol in place of methanol the separation was improved, but was accompanied by a decrease in column efficiency. The end-capping effect of the remaining surface silanols on enantiomer resolution is discussed.