A kind of hydrophilic magnetic mesoporous microsphere and its preparation method and application
A magnetic and mesoporous technology, applied in the preparation of microspheres, the preparation of peptides, magnetic materials, etc., to achieve the effects of good magnetic field sensitivity, good use value and application prospects, and strong specificity
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Embodiment 1
[0030] Example 1 Synthesis of hydrophilic magnetic mesoporous microspheres
[0031] Hydrothermal synthesis of magnetic microspheres: using 6.8 grams of FeCl 3 ·6H 2 O, add 12.0 g of sodium acetate as a dispersant, mix well in 200 mL of ethylene glycol solution, add 2.0 g of trisodium citrate dihydrate, and then transfer the solution into a closed heating vessel, and perform solvothermal reaction at 200°C , The heating time is 7 h, and the ferroferromagnetic microspheres are obtained. After the product was washed, it was vacuum dried at 60°C for 12 h.
[0032] Preparation of chloropropyl modified magnetic mesoporous microspheres: take 300 mg Fe 3 O 4 The magnetic microspheres were ultrasonically dispersed in 580 mL secondary water, and 1.0 g CTAB and 24 mg NaOH were added. In a 60°C water bath, the ethanol solution of the silane precursor (8 mL, 4 mL and 8 mL of tetraethoxysilane, chloropropyltriethoxysilane and ethanol respectively) was added dropwise with mechanical stirring. C...
Embodiment 2
[0037] Example 2 Performance Test
[0038] figure 1 In the scanning electron micrograph of the hydrophilic magnetic mesoporous microspheres synthesized in Example 1, it can be seen that the particle size of the ferroferric oxide nanoparticles is about 200 nm, and the dispersion is good.
[0039] figure 2 It is a transmission electron micrograph of the hydrophilic magnetic mesoporous microspheres obtained in Example 1. It can be seen that it has an obvious core-shell structure and the shell has a vertical ordered mesoporous structure, indicating that the magnetic nanoparticles have undergone sol-gel reaction. Successfully coated with mesoporous SiO 2 shell.
[0040] image 3 The magnetic mesoporous microspheres containing CTAB (a), chloropropyl-modified magnetic mesoporous microspheres (b), azide magnetic mesoporous microspheres (c) and hydrophilic magnetic mesoporous microspheres synthesized in Example 1 Infrared spectrum of microsphere (d). In (a) there is an obvious vibration a...
Embodiment 3
[0042] Example 3 Hydrophilic magnetic mesoporous microspheres are used for the enrichment of glycosylated peptides
[0043] Take 20 μL of the peptide mixture of 2 μg / μL horseradish peroxidase (HRP) trypsin digestion and prepare 1 mL of 40 ng / μL HRP solution (80% acetonitrile and 0.2% (v / v) )Aqueous solution of acetic acid), add 0.1 mg of hydrophilic magnetic mesoporous microspheres, shake at room temperature for 30 minutes; separate the supernatant and the microspheres enriched with glycosylated peptides under the action of a magnetic field. Wash the material with 80% acetonitrile aqueous solution (containing 0.2% (v / v) acetic acid), and then use 40 μL of 20% acetonitrile aqueous solution (containing 0.2% (v / v) acetic acid) to elute the enriched glycosylated peptides. Take 10 μL of eluate and use ESI-Q-TOF mass spectrometry to detect. As shown in Figure 5, the number of glycosylated peptides detected after enrichment has increased from 4 to 10 (the corresponding mass s...
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