• 专利标题:   Covalently organic framework modified graphene material synthesis method used for identifying human serum and circulating tumor cell samples, involves dispersing graphene sheet to concentrated nitric acid, refluxing, and centrifuging.
  • 专利号:   CN106882797-A
  • 发明人:   GAO M, WANG J, ZHANG X, LI J
  • 专利权人:   UNIV FUDAN
  • 国际专利分类:   A61K031/704, A61K047/04, A61P035/00, C01B032/194, C07K001/14, G01N030/02
  • 专利详细信息:   CN106882797-A 23 Jun 2017 C01B-032/194 201757 Pages: 16 Chinese
  • 申请详细信息:   CN106882797-A CN10027161 15 Jan 2017
  • 优先权号:   CN10027161

▎ 摘  要

NOVELTY - A covalently organic framework modified graphene material synthesis method involves dispersing 300-500 mg graphene sheet to 60-70 mL concentrated nitric acid, refluxing at 50-70 degrees C for 7-9 hours, centrifuging and separating, washing solution with deionized water to neutral, drying product at 45-50 degrees C, obtaining acidified graphene, taking 400-450 mg iron(III) chloride hexahydrate and 40-60 mL ethylene glycol, stirring, adding acidified graphene, dispersing, ultrasonicating for 1.0-2.0 hours, adding trisodium citrate, sodium acetate and polyethylene glycol, and stirring for 1.0-1.5 hours.. USE - Covalently organic framework modified graphene material synthesis method used for identifying human serum and circulating tumor cell samples (claimed). ADVANTAGE - The material has loose porous structure, large area and stable biological compatibility. It has high reaction efficiency, strong specificity and good stability. The method is low-cost, simple, has high utility and stability, and good repeatability. DETAILED DESCRIPTION - A covalently organic framework modified graphene material synthesis method comprises dispersing 300-500 mg graphene sheet to 60-70 mL concentrated nitric acid, refluxing at 50-70 degrees C for 7-9 hours, centrifuging and separating, washing solution with deionized water to neutral, drying product at 45-50 degrees C, obtaining acidified graphene, taking 400-450 mg iron(III) chloride hexahydrate and 40-60 mL ethylene glycol, stirring, adding acidified graphene, dispersing, ultrasonicating for 1.0-2.0 hours, adding trisodium citrate, sodium acetate and polyethylene glycol, stirring for 1.0-1.5 hours, carrying out hydrothermal reaction for 10-12 hours at 180-220 degrees C, cooling, separating product using magnet, washing with deionized water and absolute ethanol, drying at 45-50 degrees C to obtain magnetic graphene, taking 20-40 mg magnetic graphene, adding 1,3,5-trimethylbenzene and 1,4-dioxane solution, ultrasonicating for 0.5-1.0 hour, adding 1,4-benzene diboronic and 2,3,6,7,10,11-hexahydroxytrityl, ultrasonicating for 3-4 hours, carrying out magnetic separation, washing with acetone and ethanol, and drying at 45-50 degrees C. An INDEPENDENT CLAIM is included for glycosylated peptide separation, enrichment and mass identification method comprising taking covalently organic framework modified graphene material and target peptide solution, adding 85-95 wt.% acetonitrile /0.10-0.15 wt.% trifluoroacetic acid buffer liquid, dispersing, incubating at 37-39 degrees C, carrying out enzymolysis, centrifuging, washing 3-5 times with 85-95 wt.% acetonitrile /0.10-0.15 wt.% trifluoroacetic acid buffer liquid, eluting with 25-30 wt.% acetonitrile/0.10-0.15 wt.% trifluoroacetic acid, taking 0.8-1.2 mu L eluent point on MALDI-TOFMS target plate, drying, add 0.8-1.2 mu L of 20-25 mg/mL 2,5-dihydroxybenzoic acid solution, forming matrix thin layer, drying, and carrying out mass spectrometry analysis.