文献类型：专利

英文题名：Preparation of stationary phase of curcumin bonded silica liquid chromatogram as filling material by preparing precursor of gamma-glycidoxy propyl bonded silica and reacting precursor and curcumin under backflow temperature of methylbenzene

作者：WAN H;WEI Y;ZHANG W

机构：[1]UNIV EAST CHINA SCI & TECHNOLOGY

申请号：CN101670277-A

申请日：2009-09-23

公开日：2010-03-17

语种：英文

收录：DERWENT

摘要：NOVELTY - Preparation of stationary phase of curcumin bonded silica liquid chromatogram comprises preparing precursor of gamma -glycidoxy propyl bonded silica; reacting the precursor of gamma -glycidoxy propyl bonded silica and curcumin for 16-18 hours under the backflow temperature of methylbenzene; extracting the precursor for 9-11 hours taking methylbenzene as solvent; and repeatedly washing the precursor of gamma -glycidoxy propyl bonded silica through the methylbenzene and the acetone in turn till the filtering liquid becomes clear; and drying the solid for 15-17 hours in vacuum at 75-85 degrees C. USE - Method for preparing stationary phase of curcumin bonded silica used as filling material of high-efficiency liquid chromatography and enriching material (claimed). ADVANTAGE - The method has simple structure, moderate reacting condition, lower preparing cost and wide applicability. The ligand at the surface of the stationary phase of curcumin bonded silica has higher bonding density. Compared to traditional alkyl bonding phase, the stationary phase of curcumin bonded silica is not easy to breed germ when put for a long time for the bonded ligand has a certain anti-bacterial function so as to keep stable chromatograph performance. DETAILED DESCRIPTION - Preparation of stationary phase of curcumin bonded silica liquid chromatogram comprises: (A) under nitrogen atmosphere, ratio of activated silica: mol number of coupling agent: volume of anhydrous methylbenzene of 1: 3:10-1:4.5:15 (g:mmol:mL), under stirring state, adding the coupling agent in anhydrous methylbenzene and heating to 110-115 degrees C in oil bath; and reacting the mixture for 10-12 hours under the backflow state of methylbenzene solvent then cooling and filtering the mixture; removing the solid, the redundant coupling agent through the methylbenzene and the acetone; then drying the solid for 14-18 hours in vacuum at 55-65 degrees C to obtain precursor of gamma -glycidoxy propyl bonded silica; and (B) at a ratio of activated silica: mol number of curcumin: mol number of sodium hydride: volume of anhydrous methylbenzene is 1:1.36:1.80:10 to 1:1.44:2.20:15 (g:mmol:mmol:mL), stirring the mixture for 4-6 hours and then filtering to obtain clear liquid; adding the precursor of gamma -glycidoxy propyl bonded silica in the clear liquid under stirring; and reacting the precursor of gamma -glycidoxy propyl bonded silica for 16-18 hours under the backflow temperature of methylbenzene; and extracting the precursor of gamma -glycidoxy propyl bonded silica for 9-11 hours taking the methylbenzene as the solvent; and repeatedly washing the precursor of gamma -glycidoxy propyl bonded silica through the methylbenzene and the acetone in turn till the filtering liquid becomes clear; drying the solid for 15-17 hours in vacuum at 75-85 degrees C to prepare the stationary phase of curcumin bonded silica liquid chromatogram.