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Method for producing sub 10-nanometer calcium fluoride core-shell nanocrystal and application thereof in nuclear magnetic resonance

A technology of nanocrystals and calcium fluoride, applied in nuclear magnetic resonance/magnetic resonance imaging contrast agents, nanotechnology, calcium/strontium/barium fluoride, etc. Low relaxation rate and other problems, to achieve the effect of low cytotoxicity, low biocompatibility and good water solubility

Inactive Publication Date: 2018-01-30
ANHUI PROVINCIAL HOSPITAL
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0006] In order to solve the deficiencies in the prior art, the present invention provides a preparation method of sub-10 nanometer calcium fluoride core-shell nanocrystals and its application as a T1-type NMR contrast agent. The technical problem to be solved is the existing CaF 2 The synthesis process of the T1-based MRI contrast agent is complex, not suitable for large-scale production and preparation, and the longitudinal molar relaxation rate r 1 lower disadvantage

Method used

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  • Method for producing sub 10-nanometer calcium fluoride core-shell nanocrystal and application thereof in nuclear magnetic resonance
  • Method for producing sub 10-nanometer calcium fluoride core-shell nanocrystal and application thereof in nuclear magnetic resonance
  • Method for producing sub 10-nanometer calcium fluoride core-shell nanocrystal and application thereof in nuclear magnetic resonance

Examples

Experimental program
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Effect test

Embodiment 1

[0042] This embodiment prepares water-soluble CaF according to the following steps 2 :Yb / Er@CaF 2 :Gd core-shell nanocrystals:

[0043] a, 0.02g CaO, 0.05g YbCl 3 , 0.005g ErCl 3 Add it into 3mL 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 calcium oleate, ytterbium oleate and erbium oleate Precursor;

[0044] b. Mix 0.02g CaO with 0.05g 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 calcium oleate and gadolinium oleate precursors;

[0045] c. Dissolve 0.1g NH 4 Add 3.2mL methanol solution of F and 0.05g NaOH to the mixture of 6mL 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 ...

Embodiment 2

[0059] This embodiment prepares water-soluble CaF according to the following steps 2 :Yb,Er@CaF 2 :Gd core-shell nanocrystals:

[0060] a. Mix 0.05g CaO, 0.05g Yb(NO 3 ) 3 , 0.006g Er(NO 3 ) 3 Add it into 6mL of oleic acid, stir evenly, and then keep it warm at 150°C for 300 minutes to obtain a transparent clear solution A; naturally cool the clear clear solution A to room temperature to obtain a compound of calcium oleate, ytterbium oleate and erbium oleate Precursor;

[0061] b. Combine 0.05g CaO with 0.05g Gd(NO 3 ) 3 Add it into 6mL of oleic acid, stir evenly, and then keep it warm at 150°C for 300 minutes to obtain a clear clear solution B; naturally cool the clear clear solution B to room temperature to obtain calcium oleate and gadolinium oleate precursors;

[0062] c. Dissolve 0.1g NH 4 F and 0.2g NaOH in 13mL methanol solution were added to the mixture of 6mL oleic acid and 20mL octadecene, stirred evenly, then heated to 100°C and kept for 2h to remove methan...

Embodiment 3

[0073] This embodiment prepares water-soluble CaF according to the following steps 2 :Yb,Er@CaF 2 :Gd core-shell nanocrystals:

[0074] a. Mix 0.03g CaO, 0.05g Yb(NO 3 ) 3 , 0.005g Er(NO 3 ) 3 Add it into 4mL 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 calcium oleate, ytterbium oleate and erbium oleate Precursor;

[0075] b. Combine 0.05g CaO with 0.05g Gd(NO 3 ) 3 Add it into 4mL of oleic acid, stir evenly, and then keep it warm at 100°C for 60 minutes to obtain a transparent clear solution B; naturally cool the clear clear solution B to room temperature to obtain calcium oleate and gadolinium oleate precursors;

[0076] c. Dissolve 0.1g NH 4 F and 0.08g NaOH in 8mL methanol solution were added to the mixture of 6mL oleic acid and 10mL octadecene, stirred evenly, then heated to 70°C and kept for 1h to remove methan...

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Abstract

The invention discloses a method for producing a sub 10-nanometer calcium fluoride core-shell nanocrystal, and application thereof in nuclear magnetic resonance. The method comprises the following steps: rapidly injecting a complex of ytterbium oleate, erbium oleate and calcium oleate at high temperature under excess amount of ammonium fluoride and sodium hydroxide, to obtain a sub 10-nanometer CaF2: Yb, Er nanocrystal; then continuously rapidly injecting the complex of ytterbium oleate, erbium oleate and calcium oleate to obtain a larger-size sub10-nanometer CaF2: Yb, Er nanocrystal; rapidlyinjecting a complex of gadolinium oleate and calcium oleate at high temperature to prepare a sub 10-nanometer CaF2: Yb / Er @ CaF2: Gd core-shell nanocrystal; and performing water-soluble surface modification to obtain the water-soluble target product. The preparation method of the core-shell nanocrystal, provided by the invention, is simple, and the obtained product as a T1 nuclear magnetic contrast agent has the very high vertical molar relaxation rate r1, and has the relatively great clinical application value.

Description

technical field [0001] The invention belongs to the technical field of nanomaterial preparation and relates to a sub-10 nanometer CaF 2 :Yb / Er@CaF 2 : Preparation method of Gd nanocrystals and its application as T1 contrast agent 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 3.0~4.0mM -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] German "German Applied Chemistry" (Angew.Chem.Int.Ed., 2013, Volume 52, Pages 6671-6676) reported the synthesis of sub-10nm...

Claims

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Application Information

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IPC IPC(8): C01F11/22B82Y40/00A61K49/08A61K49/18
Inventor 徐运军刘坤闫旭董良钱海生陆杨宋永红李飞苏杨陈胜
Owner ANHUI PROVINCIAL HOSPITAL
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