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Water-soluble nayf4:yb,er@nagdf4 core-shell nanocrystals and their preparation methods and applications in nuclear magnetic resonance

A water-soluble, nanocrystalline technology, which is applied in pharmaceutical formulations, preparations for in vivo tests, emulsion delivery, etc., can solve the problems of unsuitable for large-scale production preparation, complex surface modification process, and synthesis process of T1 nuclear magnetic contrast agent Complicated problems, to achieve the effect of low biocompatibility, low cytotoxicity and good water solubility

Active Publication Date: 2019-03-08
HEFEI UNIV OF TECH
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] The present invention provides a water-soluble NaYF 4 :Yb,Er@NaGdF 4 The preparation method of core-shell nanocrystals and its application as a T1-type nuclear magnetic contrast agent, the technical problems to be solved are the shortcomings of the existing T1-type nuclear magnetic contrast agent, such as complicated synthesis process, complicated surface modification process, and unsuitable for large-scale production and preparation.

Method used

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  • Water-soluble nayf4:yb,er@nagdf4 core-shell nanocrystals and their preparation methods and applications in nuclear magnetic resonance
  • Water-soluble nayf4:yb,er@nagdf4 core-shell nanocrystals and their preparation methods and applications in nuclear magnetic resonance
  • Water-soluble nayf4:yb,er@nagdf4 core-shell nanocrystals and their preparation methods and applications in nuclear magnetic resonance

Examples

Experimental program
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Effect test

Embodiment 1

[0041] This embodiment prepares water-soluble NaYF according to the following steps 4 :Yb,Er@NaGdF 4 Core-shell nanocrystals:

[0042] a. Add 0.02g YCl 3 , 0.01g YbCl 3 , 0.0001g ErCl 3 Add it into 3.01mL of oleic acid, stir evenly, and then keep it warm at 80°C for 20 minutes to obtain a transparent clear solution A; naturally cool the clear clear solution A to room temperature to obtain a compound of yttrium oleate, ytterbium oleate and erbium oleate precursors;

[0043] b. Add 0.03g GdCl 3 Add it into 3mL of oleic acid, stir evenly, and then keep it warm at 80°C for 20 minutes to obtain a transparent clear solution B; naturally cool the clear clear solution B to room temperature to obtain the gadolinium oleate precursor;

[0044] c. Dissolve 0.1g NH 4 Add 4mL methanol solution of F and 0.02g NaOH to the mixture of 10mL oleic acid and 10mL octadecene, stir evenly, then heat to 50°C and keep it for 0.5h to remove methanol, heat to 240°C under nitrogen protection flow a...

Embodiment 2

[0057] This embodiment prepares water-soluble NaYF according to the following steps 4 :Yb,Er@NaGdF 4 Core-shell nanocrystals:

[0058] a. Mix 0.05g Y(NO 3 ) 3 , 0.01g YbCl 3 , 0.0002g Er(NO 3 ) 3 Add it into 0.3mL oleic acid, stir evenly, and then keep it warm at 150°C for 300min to obtain a transparent clear solution A; naturally cool the clear clear solution A to room temperature to obtain a compound of yttrium oleate, ytterbium oleate and erbium oleate precursors;

[0059] b. Add 0.03g Gd(NO 3 ) 3 Add it into 0.15mL oleic acid, stir evenly, and then keep it warm at 150°C for 300min to obtain a transparent clear solution B; naturally cool the clear clear solution B to room temperature to obtain the gadolinium oleate precursor;

[0060] c, 0.296g NH will be dissolved 4 F and 0.592g NaOH in 10mL methanol solution were added to the mixture of 10mL oleic acid and 10mL octadecene, stirred evenly, then heated to 100°C and kept for 2h to remove methanol, heated to 320°C u...

Embodiment 3

[0070] This embodiment prepares water-soluble NaYF according to the following steps 4 :Yb,Er@NaGdF 4 Core-shell nanocrystals:

[0071] a. Add 0.03g Y(CH 3 COO) 3 , 0.01g Yb(CH 3 COO) 3 , 0.0002g Er(CH 3 COO) 3 Add it into 1.5mL oleic acid, stir evenly, and then keep it warm at 100°C for 60 minutes to obtain a transparent clear solution A; naturally cool the clear clear solution A to room temperature to obtain a compound of yttrium oleate, ytterbium oleate and erbium oleate precursors;

[0072] b. Mix 0.05g Gd(CH 3 COO) 3 Add it into 1.5mL oleic acid, stir evenly, and then keep it warm at 100°C for 60 minutes to obtain a clear liquid B; naturally cool the clear liquid B to room temperature to obtain the gadolinium oleate precursor;

[0073] c. Dissolve 0.1g NH 4 F and 0.08g NaOH in 10mL methanol solution were added to the mixture of 10mL oleic acid and 10mL octadecene, stirred evenly, then heated to 70°C and kept for 1h to remove methanol, heated to 280°C under nitro...

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Abstract

The invention discloses water-soluble NaYF4:Yb, Er@NaGdF4 core-shell nanocrystalline as well as a preparation method and applications of the water-soluble NaYF4:Yb, Er@NaGdF4 core-shell nanocrystalline in nuclear magnetic resonance. The preparation method of the water-soluble NaYF4:Yb, Er@NaGdF4 core-shell nanocrystalline is characterized by comprising the following steps: under the condition with excessive fluorinated ammonia and sodium hydroxide, rapidly injecting a compound formed by mixing ytterbium oleate, erbium oleate and yttrium oleate at a certain ratio at high temperature, thus preparing 10-sub-nanometer NaYF4: Yb, Er nanocrystalline, further rapidly injecting a certain amount of gadolinium oleate compound at high temperature, thus preparing oil-soluble NaYF4:Yb, Er@NaGdF4 core-shell nanocrystalline with a thin shell layer, and carrying out water-soluble surface modification on the oil-soluble NaYF4:Yb, Er@NaGdF4 core-shell nanocrystalline by adopting polyethylene glycol-polyacrylic acid (PEG-PAA), thus obtaining the target product. The preparation method of the water-soluble NaYF4:Yb, Er@NaGdF4 core-shell nanocrystalline is simple, the obtained product as a T1 nuclear-magnetic contrast agent has very high longitudinal Moore relaxation rate r1, wherein r1 is 15-25 mM<-1>S<-1>, and thus the product has a great clinical application value.

Description

technical field [0001] The invention belongs to the technical field of nanomaterial preparation and relates to a water-soluble NaYF 4 :Yb,Er@NaGdF 4 Core-shell nanocrystals and their use as T1-type contrast agents in magnetic resonance imaging. Background technique [0002] Currently clinically used T1-weighted magnetic resonance imaging contrast agent Gd-DTPA (MaggenVision), its longitudinal molar relaxation rate r in a 3T magnetic field 1 Only 3.8~4.0mM -1 S -1 , and as a chelate, Gd 3+ It is easy to leak out and cause renal fibrosis. Higher longitudinal molar relaxation rate (r 1 ) T1-type MRI contrast agent can not only greatly reduce Gd 3+ The leakage can also reduce the clinical drug dose, thereby reducing the risk of renal fibrosis to a great extent, which has great clinical application potential and significance. [0003] Germany "Advanced Materials" (Advanced Materials, 2014, Volume 26, Pages 3867-3872) reported the synthesis of 2nm-sized NaGdF 4 nanodots, ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): A61K49/12A61K49/18A61K49/10
CPCA61K49/10A61K49/12A61K49/1818
Inventor 钱海生刘坤郝梨娜陆杨
Owner HEFEI UNIV OF TECH
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