Water-soluble fullerene nano-material and preparation method and applications thereof
A technology of nanomaterials and fullerenes, applied in the field of water-soluble fullerene nanomaterials and its preparation method and application, to achieve high tumor inhibition rate, good affinity, and the effect of being conducive to popularization and application
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Embodiment 1
[0052] Embodiment 1, C 70 (OH) x (Amino Acid) y Synthesis
[0053] (1) Fullerene C 70 (OH) 29 Synthesis
[0054] C in toluene solution 70 Mix with a NaOH solution with a concentration of 50%, add a small amount of phase transfer catalyst tetramethylammonium hydroxide (TBAH), stir for 24 hours, add ethanol to precipitate the product, and dialyze to remove excess NaOH to obtain the product C 70 (OH) 29 , freeze-dried and stored.
[0055] (2)C 70 (OH) 13 (CH 2 OHCHNHCOOH) 4 Synthesis
[0056] The alkali solution of NaOH and serine (wherein the mass fraction of NaOH is 33%, the molar ratio of serine and NaOH is 1:4) is mixed with ethanol, and added dropwise to C 70 (serine and C 70 In a toluene solution with a molar ratio of 100:1), stir overnight (12h), remove the upper toluene layer, and dialyze the lower layer to remove excess NaOH, freeze-dry and store.
Embodiment 2
[0057] Embodiment 2, C 70 (OH) x (Amino Acid) y Number of modified hydroxyl groups and amino acids
[0058] (1) Determination of C 70 (OH) 29 hydroxyl number
[0059] According to elemental analysis (Flash EA 1112) result: C 53.55%, H 3.19%, Nfigure 1 shown) to calculate C 70 (OH) x number of hydroxyl groups. From thermogravimetric analysis, it can be known that C 70 (OH) x The solid powder contains 11.8% water, which is about 10 water molecules. Combined with the H content in the elemental analysis, it is estimated that the H content in the hydroxyl group is 1.87%. From this, the C can be calculated. 70 (OH) x The number of hydroxyl groups is 29.
[0060] (2) Determination of C 70 (OH) 13 (CH 2 OHCHNHCOOH) 4 The number of hydroxyl and serine
[0061] According to elemental analysis (Flash EA 1112) result: C 47.99%, H 3.21%, N 2.68%, combined thermogravimetric analysis, derivative thermogravimetric analysis curve (such as figure 2 shown) to calculate C 70 (O...
Embodiment 3
[0062] Embodiment 3, the mensuration of the hydrated particle size of water-soluble fullerene nanomaterial
[0063] Get the C prepared by the embodiment of the present invention 1 in a small amount 70 (OH) 29 and C 70 (OH) 13 (CH 2 OHCHNHCOOH) 4 The powder is dissolved in water to form a dilute solution. Due to the intermolecular interaction, C 70 (OH) 29 and C 70 (OH) 13 (CH 2 OHCHNHCOOH) 4 Agglomerates into nanoparticles in water to form particles with a hydrated particle size of 1-200nm.
[0064] The hydrated particle size of the nanoparticles in pure water at pH=7.0 was measured by dynamic light scattering (DLS, Zetasizer Nano ZSP), C 70 (OH) 29 and C70 (OH) 13 (CH 2 OHCHNHCOOH) 4 The average particle diameters are 136.4±0.5nm and 134.7±0.4nm respectively, see image 3 .
[0065] A high-resolution atomic force microscope ( 4BioScience AFM) measured C 70 (OH) 29 and C 70 (OH) 13 (CH 2 OHCHNHCOOH) 4 The sizes of nanoparticles aggregated in water are ...
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