▎ 摘 要
NOVELTY - Method for synthesizing a metal-organic framework (MOF)-modified magnetic nanoprobe with an aluminum ion, as central ion involves (a) dispersing ferroferric oxide magnetic beads in n-hexane solution dissolved with graphene oxide (GO), ultrasonically dispersing and magnetically separating the material, (b) calcining the material obtained in step (a) to obtain calcined material i.e. GO@ferroferric oxide, (c) dissolving 3,5-pyrazoledicarboxylic acid and sodium hydroxide in pure aqueous solution, ultrasonically treating and preheating, (a) adding aluminum chloride hexahydrate to the solution obtained in step (c) and ultrasonically treating until dissolution and (e) dispersing the calcined material obtained in step (b) in solution obtained in step (d), reacting, magnetically separating the product, washing with deionized water and absolute ethanol, vacuum drying to obtain a MOF-modified magnetic nanoprobe with aluminum ion as the central ion. USE - The method is useful for synthesizing MOF-modified magnetic nanoprobe with an aluminum ion, as central ion is useful in selective separation, enrichment and mass spectrometry identification of glycosylated peptides and in enrichment and identification of glycopeptides in clinical serum samples and its glycosylation proteomics analysis (all claimed). ADVANTAGE - The method prepares nanoprobe, which has a large specific surface area, strong hydrophilicity and a suitable pore size and exhibits good stability in the enrichment of standard glycosylated peptide samples, excellent size exclusion effect and ultra-low sensitivity for analysis of glycosylated proteomics in clinical serum samples. DETAILED DESCRIPTION - Method for synthesizing a metal-organic framework (MOF)-modified magnetic nanoprobe with an aluminum ion, as central ion involves (a) dispersing 50-200 mg ferroferric oxide magnetic beads having size of 10-30 nm in 10-30 ml n-hexane solution dissolved with 20-50 mg graphene oxide (GO), ultrasonically dispersing for 1-4 hours and magnetically separating the material, (b) calcining the material obtained in step (a) at 400-600℃ for 2-6 hours to obtain calcined material i.e. GO@ferroferric oxide, (c) dissolving 0.5-1 g 3,5-pyrazoledicarboxylic acid and 0.2-0.5 g sodium hydroxide in 50-150 ml pure aqueous solution, ultrasonically treating for 0.5-2 hours and preheating at 100℃ for 30 minutes, (a) adding 0.8-2.1 g aluminum chloride hexahydrate to the solution obtained in step (c) and ultrasonically treating until dissolution and (e) dispersing the calcined material obtained in step (b) in solution obtained in step (d), reacting at 25-100℃ for 2-24 hours, magnetically separating the product, washing 2-5 times with deionized water and absolute ethanol, vacuum drying at 40-80℃ to obtain a MOF-modified magnetic nanoprobe with aluminum ion as the central ion, which is denoted as GO@ferroferric oxide@MOF-303. INDEPENDENT CLAIMS are included for the following: MOF-magnetic nanoprobe modified with an aluminum ion, as central ion obtained by the performing the above-mentioned method; and use of the MOF-magnetic nanoprobe modified with an aluminum ion, as central ion in selective separation, enrichment and mass spectrometry identification of glycosylated peptides and in enrichment and identification of glycopeptides in clinical serum samples and its glycosylation proteomics analysis, where the selective separation, enrichment and mass spectrometry identification of glycosylated peptides is performed by fully mixing the MOF-magnetic nanoprobe modified with an aluminum ion, as central ion with target glycosylated peptide solution, adding 80-95% acetonitrile/1-2% trifluoroacetic acid buffer, evenly dispersing, incubating in a enzymolysis instrument at -40℃, magnetically separating the magnetic probe, washing the magnetic probe 3-5 times with 80-95% acetonitrile/1-2% trifluoroacetic acid buffer, eluting with 25-30% acetonitrile/0.1-0.15% trifluoroacetic acid, spotting 0.8-1.2 μl eluate on matrix-assisted laser desorption/ionization-time of flight (MALDI-TOF) mass spectrometry (MS) target plate, natural drying, dripping 0.8-1.2 μl 15-25 mg/ml 2,5-dihydroxybenzoic acid (DHB) solution on the analyte droplet to form a thin-layer matrix and then drying for mass spectrometry analysis.