Preparation method of folic acid self-assembled water-soluble rare-earth doped up-converted nanometer material
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A technology of rare earth doping and nanomaterials, applied in the direction of luminescent materials, material excitation analysis, chemical instruments and methods, etc., can solve the problems of no targeting, poor solubility, strong toxicity, etc., achieve low cost, low synthesis temperature, The effect of simple process
Inactive Publication Date: 2015-04-15
TIANJIN NORMAL UNIVERSITY
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[0004] Before, we published the patent "Preparation method of water-soluble red and green light tunable rare earth doped up-conversion nanomaterials" (patent application number 201310403495.8, publication number CN103436263A) adopts ethylene glycol-high-purity water system, and the synthesized particles have uniform size, adjustable color, and good water solubility, but show certain defects in the later stage of cell imaging, such as poor solubility (up to 10 mg / mL) , weak fluorescence, strong toxicity and no targeting
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Embodiment 1
[0030] First, the yttrium oxide Y 2 o 3 4 mmol, ytterbium oxide Yb 2 o 3 0.9 mmol, erbium oxide Er 2 o 3 0.1 mmol (Y / Yb / Er=80 / 18 / 2), weigh the mass, put it into a 50 mL small beaker, add 10 mL concentrated nitric acid, 5 mL high-purity water, nitrate in a fume hood at 100 oC, evaporate to dryness, Add about 20 mL of high-purity water to re-dissolve the precipitated rare earth nitrate salt, transfer it to a 50 mL volumetric flask, shake it to a constant volume, and take 5 mL of the stock solution each time for experiments.
Embodiment 2
[0032]Weigh 16 mmol of NaF, put it in a 50 mL beaker, add 8 mL of diethylene glycol and 2 mL of high-purity water, 0.15 gPEI, heat and stir at 20 oC, pipette 5 mL of stock solution with a 5 mL pipette, and add dropwise to the above solution , transferred to a three-necked flask, nitrogen, and an oil bath at 200 oC for 0.5 h. Transfer to a 25 mL reaction kettle, react at 200 oC for 24 h, cool naturally, measure the pH as 8, transfer to a 5 mL centrifuge tube, centrifuge at 10000 rpm for 5 min at 10 oC, pour off the above liquid, add 3 mL of 95% (w / w) ethanol, sonicate for 15 min, continue to centrifuge, then wash with 3 mL of 95% (w / w) ethanol, 3 mL of high-purity water, transfer to a watch glass, and dry at 50 oC in vacuum .
Embodiment 3
[0034] Disperse the centrifuged and washed particles (PEI-UCNPs) in Example 2 directly in high-purity water, weigh 0.5 g of folic acid (FA), add 0.01M sodium hydroxide (NaOH) to dissolve, and shake for 15 min. 3 Centrifugal washing and drying to obtain folic acid self-assembled upconverting nanoparticles (FA-UCNPs).
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Abstract
The invention discloses a preparation method of a folic acid self-assembled water-soluble rare-earth doped up-converted nanometer material. The preparation method mainly comprises the following steps: taking 9mL of diglycol and 6mL of high-purity water as solvents, adding 1mmol of Ln(Y / Yb / Er=80 / 18 / 2), 16mmol of NaF and 0.15g of polyethyleneimine (PEI), measuring the pH which is 9, stirring and reacting for 0.5 hour in the presence of nitrogen at 200 DEG C, transferring to a reaction kettle, reacting for 24 hours at 200 DEG C, naturally cooling and centrifugally washing to obtain polyethyleneimine modified up-converted nanometer particles (PEI-UCNPs), dispersing 1g of the PEI-UCNPs in the high-purity water, adding 0.1g of folic acid, oscillating for 15 minutes, centrifugally washing, and then dispersing in the high-purity water to obtain folic acid self-assembled up-converted nanometer particles (FA-UCNPs). As the folic acid and a folic acid receptor can be specifically bound with each other, the folic acid self-assembled rare-earth doped up-converted nanometer material can be used for identifying cancer cells and applied to targeting imaging of the cancer cells.
Description
[0001] This patent is supported by the General Project 21375095 of the National Natural Science Foundation of China, the National Excellent Doctoral Dissertation Author Special Fund FANEDD-201023, the Key Project of Tianjin Applied Basic Research Program 12JCZDJC21700, the "Young and Middle-aged Backbone Innovative Talents Training Program" ZX110GG015 of Tianjin Universities and Tianjin Supported by the "Bohai Scholars" Project of Talent Introduction 5RL098 of Normal University. technical field [0002] The invention belongs to the field of preparation of fluorescent nanomaterials, in particular to a preparation method of folic acid self-assembled water-soluble rare earth doped up-conversion nanomaterials, which is applied to cell imaging. Background technique [0003] Rare earth-doped upconversion nanomaterials have many advantages that organic dyes and semiconductor quantum dots do not have, including long fluorescence lifetime without flickering, low toxicity, high fluores...
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