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Water-soluble NaYF4:Yb, Er@NaGdF4 core-shell nanocrystalline as well as preparation method and applications thereof in nuclear magnetic resonance

A water-soluble, nanocrystalline technology, used in pharmaceutical formulations, preparations for in vivo testing, emulsion delivery, etc., can solve the complex synthesis process of T1-type nuclear magnetic contrast agent, not suitable for large-scale production preparation, surface modification process complex problems, to achieve the effect of low biocompatibility, good water solubility, and low cytotoxicity

Active Publication Date: 2016-11-09
HEFEI UNIV OF TECH
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  • Abstract
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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.

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  • Water-soluble NaYF4:Yb, Er@NaGdF4 core-shell nanocrystalline as well as preparation method and applications thereof in nuclear magnetic resonance
  • Water-soluble NaYF4:Yb, Er@NaGdF4 core-shell nanocrystalline as well as preparation method and applications thereof in nuclear magnetic resonance
  • Water-soluble NaYF4:Yb, Er@NaGdF4 core-shell nanocrystalline as well as preparation method and applications thereof in nuclear magnetic resonance

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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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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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