• 专利标题:   Preparing magnetic oxide graphene based mixed semi-micelles solid phase extraction agent comprises e.g. preparing graphite oxide, preparing graphene oxide, preparing magnetic oxide graphene, preparing mixed-micelle phase extraction agent.
  • 专利号:   CN107029685-A
  • 发明人:   HE H, WU J, ZHAO H, XIAO D, PENG J
  • 专利权人:   UNIV CHINA PHARM
  • 国际专利分类:   B01J020/20, B01J020/22, B01J020/28, B01J020/281, B01J020/30, G01N030/08
  • 专利详细信息:   CN107029685-A 11 Aug 2017 B01J-020/281 201774 Pages: 10 Chinese
  • 申请详细信息:   CN107029685-A CN10044531 20 Jan 2016
  • 优先权号:   CN10044531

▎ 摘  要

NOVELTY - Preparing magnetic oxide graphene based mixed semi-micelles solid phase extraction agent comprises e.g. adding natural crystalline flake graphite and potassium permanganate into sulfuric acid/phosphoric acid mixed acid, reacting, taking out reaction liquid, diluting with distilled water, adding hydrogen peroxide, forming bright yellow solution, centrifuging, washing repeatedly with distilled water until it is neutral, drying in vacuum to constant weight to obtain graphite oxide, preparing graphene oxide, preparing magnetic oxide graphene and preparing mixed-micelle phase extraction agent. USE - The magnetic oxide graphene based mixed semi-micelles solid phase extraction agent is useful for drug enrichment and separation in biological samples or environmental samples (claimed). ADVANTAGE - The method: is simple and easy to control. The extraction agent: ensures extracting sample with large volume, which saves organic solvent, and can be reused; suitable for the quick analysis of the sample. DETAILED DESCRIPTION - Preparing magnetic oxide graphene based mixed semi-micelles solid phase extraction agent comprises (i) taking natural crystalline flake graphite and potassium permanganate, adding 100-500 ml sulfuric acid/phosphoric acid mixed acid, reacting at 40-120 degrees C, taking out the reaction liquid, diluting with distilled water, adding hydrogen peroxide, forming bright yellow solution, centrifuging, washing repeatedly with distilled water until it is neutral, drying at 60 degrees C in vacuum to constant weight to obtain graphite oxide, (ii) preparing the step (i) graphite oxide into suspension, under 25-40 KHz output power carrying out ultrasonic crushing for 1-5 hours, after ultrasonically grinding, centrifugal separating to remove thicker graphite oxide to obtain graphene oxide solution, (iii) adding graphene oxide, ferric trichloride and sodium acetate into ethylene glycol and diethylene glycol mixed solvent, ultrasonic to obtain black solution, transferring into polytetrafluoroethylene material reaction kettle, sealing, placing in the muffle furnace to react, after finishing reaction, cooling to the room temperature, washing many times with methanol and water, and vacuum drying at 60 degrees C to constant weight to obtain magnetic graphene oxide, and (iv) adding the step (iii) magnetic graphene oxide into buffer solution, adding ionic surfactant or ionic liquid, dispersing ultrasonically, under the external magnetic field separating and removing supernatant to obtain mixed semi-micelles solid phase extraction agent, where the ionic surfactant is sodium dodecyl sulfate, octadecyl trimethyl ammonium bromide or cetyltrimethylammonium bromide, the ionic liquid is imidazole ionic liquid, including 1-hexyl-3-methylimidazolium chloride, 1-hexyl-3-methylimidazolium bromide, 1-dodecyl-3-methylimidazole chloride, 1-dodecyl-3-methylimidazole bromide, 1-dodecyl-3-methylimidazolium hexafluorophosphate 1-hexadecyl-3-methylimidazole chloride or 1-hexadecyl-3-methylimidazole bromide. An INDEPENDENT CLAIM is also included for use method of magnetic oxide graphene based mixed semi-micelles solid phase extraction agent, comprising taking sample to be detected, adding magnetic oxide graphene based mixed semi-micelles solid phase extraction agent, ultrasonic treatment, vibrating to make the adsorption equilibrium, magnetic field separating to remove supernatant, eluting enriched analyte from the magnetic extractant with a suitable organic solvent, drying the eluate with nitrogen and re-dissolving in methanol, filtering and analyzing by liquid chromatography.