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Method for preparing ultra-small superparamagnetic ferriferrous oxide nanometer particles modified by lactobionic acid

A technology of ferroferric oxide and nanoparticles, which is applied in preparations for in vivo tests, pharmaceutical formulas, emulsion delivery, etc., to achieve the effects of easy operation and separation, easy operation and increased stability

Inactive Publication Date: 2015-12-23
DONGHUA UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Searching the literature at home and abroad, there is no discovery about the preparation of Fe with specific targeting ability of lactobionic acid with ultra-high relaxivity by mild reduction method. 3 o 4 Related reports of nanoprobes used in in vitro and in vivo orthotopic liver cancer tumor models for targeted MR imaging diagnosis

Method used

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  • Method for preparing ultra-small superparamagnetic ferriferrous oxide nanometer particles modified by lactobionic acid
  • Method for preparing ultra-small superparamagnetic ferriferrous oxide nanometer particles modified by lactobionic acid
  • Method for preparing ultra-small superparamagnetic ferriferrous oxide nanometer particles modified by lactobionic acid

Examples

Experimental program
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Effect test

Embodiment 1

[0044] 1.30gFeCl 3 ·6H 2 O was dissolved in 20mL of ultrapure water, transferred to a 250mL three-necked flask and stirred; after blowing nitrogen for 15 minutes, dissolved 0.2g of sodium sulfite in 10mL of ultrapure water and added to the three-necked flask, and continued stirring for 30 minutes; then 0.5g of Aqueous solution of hyperbranched polyethyleneimine PEI and 2 mL of NH 3 ·H 2 O was also added to the three-necked flask, stirred and reacted at 60-70°C for 30 minutes; then reacted at room temperature for 1.5 hours; after the reaction, magnetically separated the obtained black product, removed the supernatant, and added an appropriate amount of Ultrasonic dispersion in water, followed by magnetic separation, repeated ultrapure water washing three times to remove impurities, and then redispersed in 20mL ultrapure water to obtain PEI-coated Fe 3 o 4 (Fe 3 o 4 / PEI.NH 2 ) Nanoparticle aqueous solution.

Embodiment 2

[0046] Take 10mLFe 3 o 4 / PEI.NH 2 (77 mg) aqueous solution (Example 1) was washed with DMSO and redispersed in 10 mL of DMSO solution. Next, 2 mL of FI solution (1.79 mg) dissolved in DMSO was added to Fe 3 o 4 / PEI.NH 2 DMSO solution, stirred for 1 day, the product Fe 3 o 4 / PEI.NH 2 -FI is magnetically separated and washed with ultrapure water, then dispersed into water. Take 25μL Fe respectively 3 o 4 / PEI.NH 2 (Example 1), Fe 3 o 4 / PEI.NH 2 Put the aqueous solution of -FI in a 2mL centrifuge tube, add 700μL of ultrapure water to it, ultrasonically homogenize it, and measure the ultraviolet absorption (see figure 1 ). It can be seen from the figure that the Fe 3 o 4 / PEI.NH 2 (Curve 1) there is no obvious ultraviolet absorption peak at 400 to 600nm, while Fe 3 o 4 / PEI.NH 2 -FI (curve 2) has an obvious UV absorption peak at 500nm, which shows that FI is successfully modified to Fe 3 o 4 / PEI.NH 2 nanoparticle surface.

Embodiment 3

[0048] Mix and dissolve 5.4mg LA, 2.9mg EDC, and 1.7mg NHS in phosphate buffered saline PBS (pH=6.0), stir and activate for 2-4 hours to activate the carboxyl group of LA. Then, the above mixed solution was added to 20 mg COOH-PEG-NH 2 In the PBS (pH=6.0) solution, continue to stir the reaction for 3 days, dialyze with a dialysis bag with a molecular weight cut-off of 1000 for 3 days, and then vacuum freeze-dry to obtain COOH-PEG-LA. Take 3 mg of synthesized COOH-PEG-LA in deuterated D 2 NMR analysis was performed in O ( 1 HNMR) (see figure 2 ). It can be seen from the figure that the peaks at 3.8 and 4.3ppm prove that lactobionic acid is successfully linked to PEG, and it can be seen from the integration of the peak area that 0.7 lactobionic acid is linked to each PEG.

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Abstract

The invention relates to a method for preparing ultra-small superparamagnetic ferriferrous oxide nanometer particles modified by lactobionic acid. The method includes the steps that after ferric iron salt reacts with natrium sulfurosum, hyperbranched polyethyleneimine and ammonium hydroxide are added, and FI is added after the reaction, and Fe<3>O<4> / PEI.NH<2>-FI is obtained; LA is activated through EDS and NHS and added to a solution of COOH-PEG-NH<2>, and COOH-PEG-LA is obtained after a reaction; the COOH-PEG-LA is activated through EDC and NHS and added to the Fe<3>O<4> / PEI.NH<2>-FI, the mixture conducts a reaction and acetylated, and the ultra-small superparamagnetic ferriferrous oxide nanometer particles are obtained. The method is simple, mild in reaction condition and easy to operate; the prepared nanometer particles are small in particle size and quite high in relaxation rate, have good colloidal stability, biocompatibility and the target ability of high-expression tumor cells of a specific asialoglycoprotein receptor and have potential application value in the field of in-vivo tumor target MR imaging diagnosis.

Description

technical field [0001] The invention belongs to the field of preparation of iron ferric oxide nanoparticles, in particular to a preparation method of ultra-small superparamagnetic iron ferric oxide nanoparticles modified by lactobionic acid. Background technique [0002] Liver cancer is a common malignant tumor in my country. Its incidence rate is relatively high in China. The age of high incidence is between 40 and 50 years old. It is the second killer of all malignant tumors and seriously affects the health of the general public. For a long time, due to the poor treatment effect of liver cancer, it was even called "the king of cancer". Using contrast agents to enhance contrast and improve the level of early accurate diagnosis for surgical resection or radiotherapy and chemotherapy to remove lesions can greatly improve the survival rate of patients. In medical liver enhancement contrast, commonly used contrast agents include T 1 Gadolinium-containing contrast agents (Gd-D...

Claims

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Application Information

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IPC IPC(8): A61K49/18A61K49/12
Inventor 沈明武胡勇史向阳
Owner DONGHUA UNIV
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