葡萄糖苷特异性固相萃取固定相的合成、表征及应用

以马来酰亚胺基修饰凝胶载体,通过β-葡萄糖胺和2-亚氨基硫代烷盐酸盐将作为配基的β-葡萄糖脒连接到载体上,合成了一种葡萄糖苷特异性固相萃取固定相,并对其固相萃取性能进行了表征.该固定相对葡萄糖苷具有特异性识别,并成功用于固相萃取分离葡萄糖苷.

Preparation,Characterization and Evaluation of a New Stationary Phase for Solid-phase Extraction of Glucosides

A new solid phase extraction stationary phase for the separation and extraction of glucosides has been prepared by using a positively charged β-glucosylamidine as the ligand. β-glucosylamidine,highly potent and selective inhibitor of β-glycosidase was immobilized by a one-pot procedure involving the addition of β-glucosylamine and 2-iminothiolane·HCl simultaneously to a gel matrix modified with gamma-maleimidobutyric acid N-hydroxysuccinimide ester(GMBS) via an appropriate spacer to give a solid phase extraction stationary phase for β-glycosidase without protecting the hydroxyl and amido groups. Infrared spectroscopy,nuclear magnetic resonance spectroscopy and ultraviolet-visible spectroscopy were used to characterize the products in the course of synthesis. Results showed that by passing N-Octyl-β-D-glucopyranoside and β-D-galactopyranoside or α-D-mannopyranoside mixture directly through the new SPE stationary phase,the retention of β-D-galactopyranoside was much stronger than those of β-D-galactopyranoside and α-D-mannopyranoside. The retained glucopyranoside could only be eluted by glucose solution indicating that the binding of the glucoside was of specific nature. Mass spectroscopy and ultraviolet-visible spectroscopy were used to characterize the separated compounds. It was found that the new SPE stationary phase was specific for the recognition of glucoside and could be used for separation and extraction of glucoside.