• 专利标题:   Preparation of porous graphene-horseradish peroxidase modified glassy carbon electrode by cooling concentrated sulfuric acid in ice-water bath, stirring, adding with graphite powder, sodium nitrate and potassium permanganate and reacting.
  • 专利号:   CN105044186-A, CN105044186-B
  • 发明人:   LI L, LIU X, LIU Y, LU J, LU X
  • 专利权人:   UNIV NORTHWEST NORMAL, UNIV NORTHWEST NORMAL
  • 国际专利分类:   G01N027/327
  • 专利详细信息:   CN105044186-A 11 Nov 2015 G01N-027/327 201616 Pages: 9 Chinese
  • 申请详细信息:   CN105044186-A CN10298766 03 Jun 2015
  • 优先权号:   CN10298766

▎ 摘  要

NOVELTY - Preparation of porous graphene-horseradish peroxidase modified glassy carbon electrode includes taking concentrated sulfuric acid, cooling in ice-water bath, stirring, slowly adding graphite powder, sodium nitrate and potassium permanganate, stirring, and reacting; transferring to three-neck flask, stirring, and reacting; constantly stirring, adding deionized water, heating, adding dropwise 30% hydrogen peroxide, and stirring until no bubbles; centrifuging, washing with hydrochloric acid, washing with distilled water, and centrifuging; ultrasonically stripping and centrifuging. USE - Method for preparing porous graphene-horseradish peroxidase modified glassy carbon electrode (claimed). ADVANTAGE - The method is simple and easy to operate. The product has excellent chemical inertness and biocompatibility and good electro-catalytic activity. DETAILED DESCRIPTION - Preparation of porous graphene-horseradish peroxidase modified glassy carbon electrode comprises: (A) taking concentrated sulfuric acid, cooling at - 4 degrees C in ice-water bath, stirring, slowly adding graphite powder, sodium nitrate and potassium permanganate, stirring, and reacting at 8-12 degrees C for 2 hours; transferring to three-neck flask, stirring, and reacting at 30 degrees C for 30 minutes; constantly stirring, adding deionized water, heating to 98 degrees C for 30 minutes, adding dropwise 30% hydrogen peroxide, and stirring until no bubbles; centrifuging, washing with 5% hydrochloric acid, washing with distilled water, and centrifuging; ultrasonically stripping, centrifuging, removing lower layer, and collecting upper layer; and filtering using 0.22 mu m filter membrane, washing with water for 4 times, freeze-drying, dispersing in 1 mg/mL, drying, and standing; (B) dissolving cetyltrimethylammonium bromide in water and ultrasonically mixing with first step product for 1 hour; adding dropwise 3% ammonia solution in silver nitrate solution and dissolving until white precipitate disappears to obtain silver ammonia solution; adding dropwise previous product, stirring, reacting for 2 hours under nitrogen protection, stirring, adding aqueous sodium borohydride solution, reacting at 80 degrees C for 12 hours, and performing reduction reaction of silver ions; and filtering using 0.22 mu m filter membrane, washing with water for 4 times, and freeze-drying; (C) ultrasonically dispersing in water, adding nitric acid solution, stirring at room temperature for 4 days, and removing silver nanoparticles; and filtering using 0.22 mu m filter membrane, washing with water for 4 times, and freeze-drying; (D) successively washing with 0.30 mu m, 0.05 mu m aluminum oxide suspension, adding 95 vol.% ethanol, and ultrasonically washing twice with distilled water; inserting with 1 mM ferricyanide probe molecules and 0.1 M potassium chloride electrolyte solution in glassy carbon electrode as working electrode, platinum column as counter electrode, saturated calomel electrode as reference cyclic voltammetry electrodes of three-electrode system; and removing electrode with distilled water and drying; (E) dispensing third step product onto glassy carbon electrode, treating, and drying at room temperature; dispensing with horseradish peroxidase and drying at room temperature; (F) adding to glassy carbon electrode as working electrode, platinum column as counter electrode, saturated calomel electrode as reference cyclic voltammetry electrodes of three-electrode system, soaking in 1 mM hydrogen peroxide with saturated nitrogen and 0.2 M phosphate buffer solution, and adjusting pH to 7; and (G) drawing different modified electrodes containing 1 mM hydrogen peroxide with saturated nitrogen and 0.2 M phosphate buffer solution, and adjusting pH to 7.