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Preparation method of targeted MRI (magnetic resonance imaging) contrast medium based on folic acid modified iron oxide nanoparticles

A technology of ferric tetroxide and nanoparticles, which can be used in preparations and pharmaceutical formulations for in vivo tests, can solve problems such as no discovery, and achieve the effects of simple operation, low cost of raw materials, and high targeting.

Inactive Publication Date: 2013-06-12
DONGHUA UNIV +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] Searching domestic and foreign literatures, there is no information on the preparation of PEI-coated and FA-modified Fe by one-step hydrothermal synthesis. 3 o 4 Nanoparticles and related reports on targeted MRI studies of tumor models in vivo

Method used

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  • Preparation method of targeted MRI (magnetic resonance imaging) contrast medium based on folic acid modified iron oxide nanoparticles
  • Preparation method of targeted MRI (magnetic resonance imaging) contrast medium based on folic acid modified iron oxide nanoparticles
  • Preparation method of targeted MRI (magnetic resonance imaging) contrast medium based on folic acid modified iron oxide nanoparticles

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Embodiment 1

[0071] 1.25g FeCl 2 4H 2 Pour O into a beaker, add 7.75mL of ultrapure water, and add 6.25mL of NH 3 ·H 2 O, the above mixed solution was continuously stirred for 10 minutes under air atmosphere to fully oxidize the ferrous iron, and then the mixed solution was transferred to a high-pressure reactor. Dissolve 0.5g PEI in 5mL aqueous solution by ultrasonic, transfer it into the reaction kettle with a pipette gun, mix well with the solution in the reaction kettle, and react at 134°C for 3 hours. After the reaction was over, it was naturally cooled to room temperature, and the obtained black precipitate Fe 3 o 4 -PEI magnetic separation to remove the supernatant, add an appropriate amount of ultrapure water to ultrasonically disperse, and then magnetically separate, repeat the ultrapure water washing five times to remove impurities, and then redisperse in 20mL ultrapure water to obtain PEI coating Fe 3 o 4 Nanoparticles (Fe 3 o 4 -PEI). Take 3mL nanoparticle solution, v...

Embodiment 2

[0073] Take 17.65mg FA, 6.90mg EDC and 4.14mg NHS in a reaction flask, add 5mL DMSO to dissolve it completely, and stir for 3h to activate. Take 40mg NH 2 -PEG-COOH was dissolved in 5 mL DMSO. The above activated solution (5 mL) was then added dropwise to NH 2 -PEG-COOH in DMSO solution (5 mL), stirred for three days. Use a dialysis bag with a molecular weight cut-off of 1000 to dialyze against distilled water for three days (6 times, 2L / time) to remove by-products and impurities. Freeze-dry the product COOH-PEG-FA and store it at -20°C for later use;

[0074] FA, NH 2 The proton nuclear magnetic spectrum analysis of -PEG-COOH and the synthesized COOH-PEG-FA such as figure 2As shown, the peaks of COOH-PEG-FA appearing at 6-9ppm indicate that FA has been successfully connected to PEG. According to the calculation of the integrated peak area, 0.7 FAs were connected to each PEG.

Embodiment 3

[0076] Get the Fe prepared by Example 1 3 o 4 -PEI aqueous solution 6.24mL (30mg) was washed three times with DMSO, and then Fe 3 o 4 -PEI was redispersed in 6 mL DMSO, then a solution of FI (0.84 mg) dissolved in 2 mL DMSO was added dropwise to the above 6 mL Fe 3 o 4 -In the DMSO solution of PEI, after stirring for one day, remove the supernatant by magnetic separation, add an appropriate amount of ultrapure water for ultrasonic dispersion, and then magnetic separation, repeat the pure water washing 3 times in this way to remove impurities, and then redisperse in 10mL DMSO , the product Fe is obtained 3 o 4 -PEI-FI. Take 25μL Fe respectively 3 o 4 - PEI (Example 1), FI and Fe 3 o 4 - Put the DMSO solution of PEI-FI (Example 3) in a 2mL centrifuge tube, add 700μL of ultrapure water to it, ultrasonically uniform, measure the UV absorption (see attached image 3 ). The results of UV-Vis spectroscopy test showed that Fe 3 o 4 -PEI has no obvious ultraviolet absorpt...

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Abstract

The invention relates to a preparation method of a targeted MRI (magnetic resonance imaging) contrast medium based on folic acid modified iron oxide nanoparticles. The method comprises the following steps of: connecting FA to NH2-PEG-COOH to form COOH-PEG-FA; synthesizing PEI coated Fe3O4 nanoparticles (Fe3O4-PEI) by a hydrothermal method; performing surface modification on the Fe3O4-PEI nanoparticles by use of fluorescein isothiocyanate (FI); connecting COOH-PEG-FA to the surface of the Fe3O4 nanoparticles; and finally performing acetylation modification of the residual PEI aminos on the surface of the Fe3O4 nanoparticles to improve the biocompatibility for MRI diagnosis. The preparation method provided by the invention has simple technology and mild reaction conditions, and is easy to operate; and the prepared Fe3O4 magnetic nanoparticles have good colloidal stability, biocompatibility and tumor targeting performance as well as potential application value in the field of in-vivo tumor targeted diagnosis.

Description

technical field [0001] The invention belongs to the field of preparation of nuclear magnetic resonance imaging contrast agents, in particular to a preparation method of a targeted MRI contrast agent based on folic acid-modified iron ferric oxide nanoparticles. Background technique [0002] Malignant tumors have always been the number one killer of human life, with the characteristics of high mortality, difficult treatment and rapid deterioration. Therefore, early diagnosis and specific treatment of tumors are particularly important. At present, there are various methods for tumor detection, mainly including: ultrasound imaging, CT imaging, nuclear medicine PET imaging and magnetic resonance imaging (MRI). With the development of nuclear magnetic resonance technology, the scanning time is gradually shortened, the resolution is gradually improved, and the detection of small lesions is more accurate, which also makes nuclear magnetic resonance imaging technology a new disease ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): A61K49/12A61K49/10
Inventor 沈明武李静超蔡红东史向阳张贵祥郑林丰
Owner DONGHUA UNIV
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