用反相高效液相色谱法分析及反相固相萃取法纯化 - 四（对羟基苯基）间苯二酚杯芳烃及其立体异构体。

Analysis by RP-HPLC and Purification by RP-SPE of the -Tetra(-hydroxyphenyl)resorcinolarene and Stereoisomers.

作者信息

Castillo-Aguirre Alver A, Rivera Monroy Zuly Jenny, Maldonado Mauricio

机构信息

Departamento de Química, Facultad de Ciencias, Universidad Nacional de Colombia-Sede Bogotá, Bogota 11001, Colombia.

出版信息

J Anal Methods Chem. 2019 Apr 16;2019:2051282. doi: 10.1155/2019/2051282. eCollection 2019.

DOI:10.1155/2019/2051282

PMID:31143485

原文链接:https://pmc.ncbi.nlm.nih.gov/articles/PMC6501146/

Abstract

A method for the separation of stereoisomer mixture of the octol -tetra(-hydroxyphenyl)calix[4]resorcinarene that was obtained by an acid cyclocondensation reaction between resorcinol and benzaldehyde is reported in this paper. A crude product from octol formation reaction was analyzed by reverse-phase high-performance liquid chromatography (RP-HPLC), and two well-resolved signals corresponding to the and isomers were found. A reverse phase in solid-phase extraction (RP-SPE) protocol allowed the separation of the two stereoisomers with high purity of each isomer. Finally, the crude and purified stereoisomers were characterized by using FT-IR, H-NMR, and C-NMR techniques, confirming the chemical identity of the two isomers and the efficiency in the separation process.

摘要

本文报道了一种分离八醇-四（对羟基苯基）杯[4]间苯二酚芳烃立体异构体混合物的方法，该混合物通过间苯二酚与苯甲醛之间的酸环缩合反应获得。通过反相高效液相色谱（RP-HPLC）分析八醇形成反应的粗产物，发现了对应于两种异构体的两个分离良好的信号。固相萃取（RP-SPE）方案中的反相模式实现了两种立体异构体的分离，且每种异构体的纯度都很高。最后，使用傅里叶变换红外光谱（FT-IR）、氢核磁共振（H-NMR）和碳核磁共振（C-NMR）技术对粗产物和纯化后的立体异构体进行了表征，证实了两种异构体的化学特性以及分离过程的有效性。