Preparation method of Fe3O4 nano-magnetic resonance contrast medium material
A magnetic resonance contrast agent, nanotechnology, applied in the direction of nuclear magnetic resonance/magnetic resonance imaging contrast agent, etc., to achieve the effects of good biocompatibility, short response time and low price
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Embodiment 1
[0039] Weigh sodium citrate (0.2g, 0.68mmol) and dissolve it in 20ml ethylene glycol, add anhydrous FeCl after ultrasonic stirring to dissolve 3 (0.3244g, 2.0mmol), after ultrasonic dissolution, add 1.20g CH 3 COONa·3H 2 O (9mmol), dissolved by ultrasound, stirred for 30min, transferred the solution to a 50ml reactor, and reacted at 200°C for 10h. After cooling, the precipitate was washed three times with ethanol and deionized water, and freeze-dried to obtain superparamagnetic Fe 3 o 4 Magnetic nanoparticles, water soluble. The particle size is 200-300nm, as shown in the transmission electron microscope figure 1 As shown, the XRD spectrum is as figure 2 shown.
Embodiment 2
[0041] Prepare the NaOH solution of 10ml 5mol / L, and transfer in the 100ml single-necked round bottom flask, add the dry good Fe in 60mg embodiment 1 3 o 4 Magnetic nanoparticles, stirred for 2h, then added dropwise 6ml epichlorohydrin (55mmol) under the protection of nitrogen, stirred for 24h under the protection of nitrogen, the precipitate was taken and washed three times with deionized water. After washing, redissolve the particles in 25ml of deionized water, add 12ml of ammonia water (concentration: 25wt%-28wt%, about 0.2mol), and stir at 37°C for 36h. Washed three times with ethanol and deionized water respectively, and freeze-dried to obtain amino-functionalized superparamagnetic Fe 3 o 4 Nanoparticle Fe 3 o 4 NH 2 .
Embodiment 3
[0043] Folic acid (FA) (2.5mg, 1.08×10 -5 mol) was dissolved in 20ml dimethyl sulfoxide (DMSO), then 1-ethyl-(3-dimethylaminopropyl) carbodiimide hydrochloride (EDC·HCl) and N-hydroxysuccinimide were added Amine (NHS), FA, EDC and NHS were input according to the feed ratio (molar ratio) of 1:1:2.5, and stirred for 3h under the protection of nitrogen. Then the amino functionalized dry good Fe in embodiment 2 3 o 4 Weigh 40mg and dissolve it in 10ml DMSO, then add it dropwise to the above solution, stir overnight under nitrogen protection, finally wash with phosphate buffer saline (PBS) three times, and freeze-dry to obtain the superciliary substance attached to the target substance. Magnetic Fe 3 o 4 Nano-magnetic resonance contrast agent material Fe 3 o 4 NH 2 Fa.
[0044] The Fe obtained by the above method 3 o 4 Nano-magnetic resonance contrast agent material, the shape is spherical, the particle size is 200-300nm, and Fe with a particle size of 200-300nm 3 o 4 M...
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