• 专利标题:   Preparing functional drug-loading material used for preparing composite medicine carrying system, involves adding silicon dioxide powder in water to get silicon dioxide dispersion, and under stirring, dripping into graphene oxide dispersion.
  • 专利号:   CN108578703-A
  • 发明人:   LIANG C, SONG J, GAO W, ZHANG Y
  • 专利权人:   UNIV HEBEI TECHNOLOGY
  • 国际专利分类:   A61K047/02, A61K047/04, A61K047/69, A61K047/26, C01G049/08, B82Y030/00
  • 专利详细信息:   CN108578703-A 28 Sep 2018 A61K-047/02 201878 Pages: 11 Chinese
  • 申请详细信息:   CN108578703-A CN10511799 25 May 2018
  • 优先权号:   CN10511799

▎ 摘  要

NOVELTY - Preparing functional drug-loading material involves adding silicon dioxide powder having the grain diameter of 100-500 nano-meter into the water to prepare silicon dioxide dispersion from 10-80 mg/mL, then under the stirring, dripping the silicon dioxide dispersion liquid into the graphene oxide dispersion, then putting the mixed system into the ultrasonic cell crusher to ultrasound for 40-90 minutes, in which the volume ratio of graphene oxide dispersion, silicon dioxide dispersion is 3:1, and the graphene oxide dispersion concentration is 1-6 mg/mL, then using a spray dryer for granulation, under the temperature of 160-240 degrees C, rate of 4.0-8.0 mL/minutes and frequency of 8-20 seconds/operation to obtain blackberry like graphene oxide nano-shell without removing the silicon dioxide template having the grain size range is 500 nano-meter to 10 microns, then placing the obtained substance in the vacuum tubular furnace to reduce the graphene oxide under the protection of argon gas. USE - Method for preparing functional drug-loading material used for preparing composite medicine carrying system (claimed). ADVANTAGE - The method for preparing functional drug-loading material with high drug loading rate. DETAILED DESCRIPTION - The preparation method of the functional drug-loading material further involves keeping at 300-900 degrees C for 1-3 hours, then putting the obtained substance into 8-12% hydrofluoric acid solution to soak for 18-90 hours, and centrifuging and washing with deionized water so that the pH value is 7, at last vacuum drying for 6-12 hours to obtain the blackberry like graphene nano-shell removed silicon dioxide, in the washing process, the centrifugal speed is 4000-9000 revolutions/minute and the time is 6-12 minutes, then adding polyethyleneimine (PEI) in 60-70 degrees C of polyethylene glycol (PEG), then raising to 78-85 degrees C, then adding iron acetylacetonate , then keeping the temperature for 5-15 minutes, then heating to 220-300 degrees C and keeping the temperature for 0.5-2 hours, then cooling naturally to 60 degrees C, taking out the reaction solution, orderly washing by toluene and acetone, finally dissolving the graphene nano-shell in the de-ionized water to obtain the graphene nano-shell solution, adding Tween (RTM: non-ionic surfactant) 80 into the graphene nano-shell solution, then putting in shaking table hatching for 40-80 minutes, then using a centrifuge free of Tween 80 is separated, and then dialyzing for 5 days to thoroughly remove free Tween 80 to obatin modified graphene nano shell, in which the mass ratio of polyethylene glycol, polyethylene imine (PEI) and iron acetylacetonate is 15:0.3:0.7, concentration of the graphene nano-shell solution is 8-12 mg/mL, and every 40 mL graphene nano-shell solution added with 0.1-0.5 g Tween 80, then mixing the ferric chloride hexahydrate and ferrous chloride tetrahydrate into the water to obtain the mixed solution, in which the molar ratio of ferric cation and ferrous cation in mixed solution is 0.5-2:1, in the mixed solutionof ferric cation and ferrous cation concentration is 0.08-0.15 moles/L, dropping 0.1-0.2 moles/L sodium hydroxide solution into the mixed solution under the water bath condition of 50 degrees C until it becomes orange, continuing to drip sodium hydroxide, changing start to green until it becomes black suspension, using centrifuge after washing by ethanol and de-ionized water, putting into 40-80 degrees C of blast drying box to dry, then dissolving the graphene nano-shell and magnetite nano-particles into the de-ionized water, using ultrasonic machine for ultrasonic uniformly, centrifuging the solution at 12000-14000 revolutions/minute for 10-30 minutes and washing by using ethanol and deionized water respectively, then putting the precipitates in the oven to dry to obtain the magnetic graphene nano-shell, in which the mass ratio of the material of graphene nano-shell and magnetite nano-particles is 2-3:1, and the 0.12 g oxidized graphene nano shells are added in every 100 mL water. An INDEPENDENT CLAIM is included for a method for using functional drug-loading material, which involves: (A) dissolving the magnetic graphene nano-shell and medicine doxycycline in phosphate-buffered saline solution having the pH value of 7.0-7. 4; (B) performing ultrasonic treatment for 0.5-1.5 hours; (C) stirring for 12-16 hours at room temperature; (D) centrifuging at 12000-14000 revolutions/minute for 10-30 minutes under the condition of upper centrifugal (multiple centrifugal removing unsupported doxorubicin hydrochloride); and (E) freeze-drying the centrifugal precipitate at (-)45-(-)42 degrees C for 2-3 days to obtain medicine-carrying magnetic graphene composite, in which the material mass ratio of the raw materials of the magnetic graphene nano-shell and medicine doxycycline is 0.2-0.8:1, and the 0.015 g magnetic graphene nano-shells are added into each 100 mL phosphate-buffered saline solution.