• 专利标题:   Separating and purifying aucubin by imprinting modified composite material comprises synthesizing vinylmodified graphene oxide by adding graphene nano sheet into water-ethanol mixed solution and ultrasonically stirring.
  • 专利号:   CN112266452-A
  • 发明人:   LI H, MAO L, LUO X, XU G, LI K
  • 专利权人:   UNIV JISHOU
  • 国际专利分类:   B01D015/08, B01J020/26, B01J020/30, C08F212/36, C08F220/54, C08F220/56, C08F222/14, C08F292/00, C08J009/26
  • 专利详细信息:   CN112266452-A 26 Jan 2021 C08F-292/00 202125 Pages: 6 Chinese
  • 申请详细信息:   CN112266452-A CN11235572 09 Nov 2020
  • 优先权号:   CN11235572

▎ 摘  要

NOVELTY - Separating and purifying aucubin by imprinting modified composite material comprises (1) synthesizing vinylmodified graphene oxide by adding 200 mg graphene nano sheet into 10-15 ml water-ethanol mixed solution (1: 1, V/V), ultrasonically stirring for 60 minutes, adding aqueous ammonia to adjust the solution to weak alkaline, slowly dropping in the 6-12 ml of 20 minutes 3-methyl propylene acyloxy-propyl-trimethoxy silane, stirring uniformly, reacting for 24 hours at 60 degrees C, cooling, centrifuging and separating solid, orderly using 20 mL ethanol and de-ionized water to wash for 3 times, the obtained solid at 50 degrees C, vacuum drying box 12 hours to obtain vinyl modified graphene oxide, (2) preparing temperature-sensitive peach leaf coral aglycon imprinting modified graphene oxide by weighing 2.0-5.0 mmol peach leaf coral glycoside, dissolving in 20-30 solution of acetonitrile/methanol (3: 1, V/V) containing 0.2% acetic acid in the mixture solution. USE - The method is useful for Separating and purifying aucubin by imprinting modified composite material. ADVANTAGE - The imprinted composite material has temperature-sensitive adsorption and desorption capability, enrichment capability and can be used repeatedly and has good application prospect. DETAILED DESCRIPTION - Separating and purifying aucubin by imprinting modified composite material comprises (1) synthesizing vinylmodified graphene oxide by adding 200 mg graphene nano sheet into 10-15 ml water-ethanol mixed solution (1: 1, V/V), ultrasonically stirring for 60 minutes, adding aqueous ammonia to adjust the solution to weak alkaline, slowly dropping in the 6-12 ml of 20 minutes 3-methyl propylene acyloxy-propyl-trimethoxy silane, stirring uniformly, reacting for 24 hours at 60 degrees C, cooling, centrifuging and separating solid, orderly using 20 mL ethanol and de-ionized water to wash for 3 times, the obtained solid at 50 degrees C, vacuum drying box 12 hours to obtain vinyl modified graphene oxide, (2) preparing temperature-sensitive peach leaf coral aglycon imprinting modified graphene oxide by weighing 2.0-5.0 mmol peach leaf coral glycoside, dissolving in 20-30 solution of acetonitrile/methanol (3: 1, V/V) containing 0.2% acetic acid in the mixture solution, adding 8-15 mmol acrylamide and 10-30 mmol N-isopropylacrylamide, stirring, allowing to stand for 30 minutes, adding 10-15 mmol glycol dimethacrylate and 20-40 mmol benzene, mixing uniformly, adding 50 mg benzophenone, stirring, introducing argon gas for 15 minutes, adding 120-120 nm vinyl modified graphene oxide, ultrasonic processing for 10 minutes, vacuum sealing, adding the reaction system in ultraviolet lamp to irradiate for 36 hours at room temperature, absorbing the supernatant, using 0.45 um micro-porous filter film to filter, extracting collected solid by 30 ml methanol-acetic acid (9: 1, V/V), 30 ml methanol and 30 ml tetrahydrofuran for 2 times, each time for 2 hours, filtering, vacuum drying to obtain the temperature sensitive peach leaf coral aglycon modified graphene oxide composite material, (3) separating and purifying the aucubin by adding 1.2-3.0 g temperature-sensitive peachleaf coral aglycon modified graphene oxide composite material into the solid phase extraction pipe, at 25 degrees C, orderly using 15 ml methanol-water (1: 1, V/V) mixed solution and 10 ml acetonitrile washing the residual compound in the extraction column and balancing, carrying out solid phase extraction, controlling the solid phase extraction column temperature is 40-45 , flowing 12-18 ml bark seed ethanol extract concentrated solution containing aucubin through the composite material adsorbent layer, collecting the effluent and analyzing the leakage target concentration, calculating the sample amount on the extraction column, reducing the extraction column temperature is 25-35 degrees C, orderly using 10-15 ml acetonitrile, 10-15 ml acetonitrile-acetone (1: 1, V/V) mixed solution and 10-15 ml ethyl acetate-ethanol (95: 5, V/V) mixed solution to wash the impurity compound absorbed in the extraction column, using 30-50 ml aqueous solution to elute, collecting the ethanol eluent, vacuum extracting and distilling most of the solvent, dissolving in 3-8 ml de-ionized water, and placing 2-5 low temperature to re-crystallize to obtain the peachleaf coral glycoside crystal with purity of 75-85.