Synthesis method and application of a magnetic metal-organic framework composite material
An organic framework and composite material technology, applied in advanced nanomaterials and nanometer fields, can solve the problems of limited enrichment of phosphorylated peptides, poor specific surface area, etc., and achieve strong adsorption, high magnetic responsiveness, and good magnetic responsiveness.
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Embodiment 1
[0028] Example 1: Synthesis of a metal-organic framework composite material with magnetic microsphere ferric oxide coated polydopamine and zirconium ion as the central metal ion
[0029] (1) 1.35g ferric chloride hexahydrate (FeCl 3 ·6H 2 O) Dissolve in 75mL of ethylene glycol, stir magnetically until clarified, add 3.6g sodium acetate, stir until dissolved, continue stirring for 0.5h, sonicate for 5 minutes, transfer to a hydrothermal reaction kettle, and heat at 200°C for 16 hours. The reactor was taken out and cooled for 10 hours; the magnetic balls obtained by the reaction were poured out from the reactor, and washed 5 times with deionized water. Dry under vacuum at 50°C.
[0030] (2) Prepare tris-hydrochloric acid (Tris-HCl) buffer solution (solvent is deionized water, pH=8.5), and disperse 0.1 g of magnetic balls obtained in step (1) in 80 mL of Tris-HCl buffer solution , sonicated for several minutes, added 0.4 g of dopamine hydrochloride, and mechanically stirred at...
Embodiment 2
[0036] Example 2: The magnetic microsphere ferric oxide obtained in Example 1 is coated with polydopamine and a metal-organic framework composite material with zirconium ion as the central metal ion as a solid phase microextraction adsorbent for low concentration β-casein Enrichment of enzymatic hydrolyzate and detection by MALDI-TOFMS.
[0037] (1) Preparation of standard proteolysis solution: Accurately weigh 2mg of standard protein β-casein and dissolve in 25mM ammonium bicarbonate buffer, boil for 10 minutes, dilute to 0.2mg / mL with 25mM ammonium bicarbonate buffer, and then follow the Add appropriate amount of trypsin (trypsin) to the protein ratio of 1:40, and enzymatically hydrolyze at 37°C for 16 hours.
[0038] (2) Enrichment of the sample: Dilute the standard protein hydrolysis solution with 25mM ammonium bicarbonate buffer to a concentration of 100nM or 10nM, take 1μL of the dilution of the enzyme hydrolysis solution and add it to 200μL of 50% acetonitrile / 0.1% trif...
Embodiment 3
[0042] Example 3: Synthesis of a metal-organic framework composite material with magnetic microsphere ferric oxide coated with polydopamine and zirconium ion as the central metal ion
[0043] (1) 1.0g ferric chloride hexahydrate (FeCl 3 ·6H 2 O) Dissolve in 55mL of ethylene glycol, stir magnetically until clarified, add 3.0g sodium acetate, stir until dissolved, continue stirring for 0.5h, sonicate for 5 minutes, transfer to a hydrothermal reaction kettle, and heat at 190°C for 18 hours. The reactor was taken out and cooled for 12 hours; the magnetic balls obtained by the reaction were poured out from the reactor, and washed 9 times with deionized water. Dry under vacuum at 60°C.
[0044] (2) Prepare tris-hydrochloric acid (Tris-HCl) buffer solution (solvent is deionized water, pH=8.5), and disperse 0.05 g of magnetic balls obtained in step (1) in 40 mL of Tris-HCl buffer solution , sonicated for several minutes, added 0.2 g of dopamine hydrochloride, and mechanically stirr...
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