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Magnetic rod-shaped nano-hydroxyapatite material and preparation method thereof

A nano-hydroxyapatite, magnetic rod technology, applied in nanotechnology, chemical instruments and methods, phosphorus compounds, etc., can solve the problems of difficult size regulation, poor dispersion, and difficult to control the synthesis of HAP nanoparticles, and achieve size The effect of uniformity, good dispersion and mild reaction process

Active Publication Date: 2019-03-08
NANJING GENERAL HOSPITAL NANJING MILLITARY COMMAND P L A
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Nano-hydroxyapatite materials for T1 magnetic resonance imaging are all prepared by precipitation method, and the synthesis of HAP nanoparticles is not easy to control, it is difficult to control the size, and the dispersion is poor

Method used

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  • Magnetic rod-shaped nano-hydroxyapatite material and preparation method thereof
  • Magnetic rod-shaped nano-hydroxyapatite material and preparation method thereof
  • Magnetic rod-shaped nano-hydroxyapatite material and preparation method thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0034] Mix sodium oleate, ethanol and oleylamine at a ratio of 1:3:1 to obtain 20 mL of mixed solution A, add 10 mL of calcium chloride aqueous solution (concentration is 0.1 mol / L), and stir at 600 rpm for 30 minutes to obtain mixed solution B Add 10mL disodium hydrogen phosphate solution (concentration is 0.06mol / L) again, obtain mixed solution C with 600 revs / min stirring 30 minutes, keep reaction system pH value 10.0 by adding NaOH aqueous solution in stirring process. Transfer the mixed solution C to a sealed reaction kettle and react at 160°C for 8 hours; the reaction product is cooled to room temperature, precipitated by centrifugation, and washed with a mixed solution of cyclohexane and ethanol at a volume ratio of 2:1 to remove organic impurities , and finally vacuum-dried to obtain a magnetic rod-shaped nano-hydroxyapatite material.

[0035] figure 1 It is the transmission electron micrograph of the magnetic rod-shaped nano-hydroxyapatite made under the process cond...

Embodiment 2

[0037] Mix sodium oleate, ethanol and oleylamine in a ratio of 1:3:1 to obtain 20mL mixed solution A; prepare an aqueous solution of calcium chloride and gadolinium salt, wherein the concentration of calcium chloride is 0.1mol / L, and the concentration of gadolinium chloride Is 0.002mol / L (the molar ratio of gadolinium ion and calcium ion is 0.02), the aqueous solution 10mL of calcium chloride and gadolinium salt is added in the mixed solution A, stirs 30 minutes with 600 rev / min to obtain mixed solution B; 10 mL of disodium hydrogen phosphate solution (concentration is 0.06 mol / L), was stirred at 600 rpm for 30 minutes to obtain mixed solution C, and the pH value of the reaction system was kept at 10.0 by adding NaOH aqueous solution during the stirring process. Transfer the mixed solution C to a sealed reaction kettle and react at 160°C for 8 hours; the reaction product is cooled to room temperature, precipitated by centrifugation, and washed with a mixed solution of cyclohexa...

Embodiment 3

[0042]Mix sodium oleate, ethanol and oleylamine in a ratio of 1:3:1 to obtain 20mL mixed solution A; prepare an aqueous solution of calcium chloride and gadolinium salt, wherein the concentration of calcium chloride is 0.1mol / L, and the concentration of gadolinium chloride Is 0.005mol / L (the molar ratio of gadolinium ion and calcium ion is 0.05), the aqueous solution 10mL of calcium chloride and gadolinium salt is added in the mixed solution A, stirs with 600 revs / min for 30 minutes to obtain mixed solution B; 10 mL of disodium hydrogen phosphate solution (concentration is 0.06 mol / L), was stirred at 600 rpm for 30 minutes to obtain mixed solution C, and the pH value of the reaction system was kept at 10.0 by adding NaOH aqueous solution during the stirring process. Transfer the mixed solution C to a sealed reaction kettle and react at 160°C for 8 hours; the reaction product is cooled to room temperature, precipitated by centrifugation, and washed with a mixed solution of cyclo...

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Abstract

The invention discloses a magnetic rod-shaped nano-hydroxyapatite material and a preparation method thereof. The preparation method comprises steps of uniformly mixing sodium oleate, ethanol, and oleylamine so as to obtain a mixed solution A, then adding a calcium chloride aqueous solution, reacting for 30 minutes whilestirring so as to obtain a mixed solution B, then adding a phosphate aqueous solution, continuing reacting for 30 minutes while stirring so as to obtain a mixed solution C, transferring the mixed solution C to a sealed reaction kettle, and reacting for 8 hours at 160 DEG C; cooling a reactant to room temperature, separating precipitates through centrifuging, washing to remove organic impurities, and finally vacuum drying to obtain the magnetic rod-shaped nano-hydroxyapatitematerial. The reaction process is mild, the size of the synthesized rod-shaped nano-hydroxyapatite is controlled through amount of doped gadolinium, and the prepared magnetic rod-shaped nano-hydroxyapatite is uniform in size and has high dispersibility. Compared with commercial Gd-DTPA contrast agent, the magnetic rod-shaped nano-hydroxyapatite material has better magnetic resonance imaging performance and is non-toxic, thereby having a bright application prospect in the biomedical field.

Description

technical field [0001] The invention relates to a magnetic rod-shaped nano-hydroxyapatite material and a preparation method thereof, belonging to the field of inorganic material preparation. Background technique [0002] Hydroxyapatite (Ca 10 (PO 4 ) 6 (OH) 2 ,HAP) as a bone substitute material is considered as an important biomaterial because of its excellent biocompatibility, bioactivity and non-toxicity. In addition, various dopants can be easily doped into the lattice of HAP, so that HAP can be used in medical applications such as bioimaging. [0003] Magnetic resonance imaging (MRI) has become one of the commonly used clinical imaging methods due to its advantages of high soft tissue contrast, deep penetration depth, non-ionizing radiation, and multi-planar reconstruction capabilities. Currently, only gadolinium chelates such as gadopentetate meglumine (Gd-DTPA) are used as T1 contrast agents. However, these gadolinium chelates can induce nephrogenic systemic fibr...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B25/32B82Y40/00
CPCB82Y40/00C01B25/325C01P2002/72C01P2002/85C01P2004/04C01P2004/16
Inventor 刘莹卢光明王守巨唐玉霞滕兆刚田迎
Owner NANJING GENERAL HOSPITAL NANJING MILLITARY COMMAND P L A
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