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Coprecipitation method for preparing methotrexate/ layered double hydroxides nanocomposite material

A nanocomposite material, methotrexate technology, applied in the field of co-precipitation method to prepare methotrexate/hydrotalcite-like nanocomposite materials, can solve the problems of difficult control of particle size distribution, easy agglomeration, etc., and achieve reliable preparation method, Good reproducibility and less contamination

Inactive Publication Date: 2012-08-15
江苏顺德缘文化科技股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the MTX / LDHs nanocomposites prepared by the traditional co-precipitation method have disadvantages such as difficult to control the particle size distribution and easy agglomeration, which have a certain impact on its practical application.

Method used

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  • Coprecipitation method for preparing methotrexate/ layered double hydroxides nanocomposite material
  • Coprecipitation method for preparing methotrexate/ layered double hydroxides nanocomposite material
  • Coprecipitation method for preparing methotrexate/ layered double hydroxides nanocomposite material

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] 1) Weigh 0.7692 g Mg(NO 3 ) 2 ?6H 2 O and 0.5627 g Al(NO 3 ) 3 ?9H 2 O, dissolved in 20 mL PEG-400 / water solvent, where, M 2+ / M3+ =2:1, the volume ratio of PEG-400 and water is: V PEG-400 / V 水 =1:3, the metal salt mixed solution is obtained;

[0035] 2) Weigh 0.3408g of MTX, dissolve it in 15 mL of 10% NH 3 ?H 2 O solution;

[0036] 3) Add the MTX mixed solution obtained in step 2) into a closed container with a constant temperature of 60°C, blow nitrogen gas for 4 minutes, and stir at a constant speed at the same time, the stirring rate is 800r / min;

[0037] 4) Add the metal salt mixed solution obtained in step 1) dropwise to the MTX mixed solution treated in step 3) at a dropping rate of 0.05 ml / s;

[0038] 5) Add dropwise 10wt% ammonia solution to adjust the pH=9.5 of the mixed solution obtained in step 4);

[0039] 6) After the pH value of the mixed solution in step 5) is constant, start timing. After 0.5 hours, cool the mixed solution to room tempera...

Embodiment 2

[0046] 1) Weigh 1.3387 g Zn(NO 3 ) 2 ?6H 2 O and 0.5627 g Al(NO 3 ) 3 ?9H 2 O, dissolved in 25 mL PEG-300 / water solvent, where, M 2+ / M 3+ =3, the volume ratio of PEG-300 and water is: V PEG-300 / V 水 =1:2, the metal salt mixed solution is obtained;

[0047] 2) Weigh 0.5453 g of MTX and dissolve it in 10 mL of 5% NaOH solution;

[0048] 3) Add the MTX mixed solution obtained in step 2) into a closed container with a constant temperature of 70°C, blow nitrogen gas for 2 minutes, and stir at a constant speed at the same time, the stirring rate is 600r / min;

[0049] 4) Add the metal salt mixture obtained in step 1) dropwise to the MTX mixed solution treated in step 3) at a dropping rate of 4 ml / s;

[0050] 5) Add dropwise 5% NaOH solution to adjust the pH=8 of the mixed solution obtained in step 4);

[0051] 6) After the pH value of the mixed solution in step 5) is constant, start timing. After 3 hours, cool the mixed solution to room temperature and pour it into a ce...

Embodiment 3

[0055] 1) Weigh 1.538g Mg(NO 3 ) 2 ?6H 2 O and 0.6060 g Fe(NO 3 ) 3 ?9H 2 O, dissolved in 15 mL PEG-600 / water solvent, where, M 2+ / M 3+ =4, the volume ratio of PEG-600 and water is: V PEG-600 / V 水 =1:4, the metal salt mixed solution is obtained;

[0056] 2) Weigh 0.2045 g of MTX and dissolve it in 25 mL of 20% methylamine solution by mass percent;

[0057] 3) Add the MTX mixed solution obtained in step 2) into a closed container with a constant temperature of 50°C, blow nitrogen gas for 7 minutes, and stir at a constant speed at the same time, the stirring rate is 1000r / min;

[0058] 4) Add the metal salt mixture obtained in step 1) dropwise to the MTX mixed solution treated in step 3) at a dropping speed of 2 ml / s;

[0059] 5) Add 20% methylamine solution dropwise to adjust the pH of the mixed solution obtained in step 4) to 11;

[0060] 6) After the pH value of the mixed solution in step 5) is constant, start timing. After 5 hours, cool the mixed solution to ro...

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Abstract

The invention discloses a coprecipitation method for preparing a methotrexate / layered double hydroxides (MTX / LDHs) nanocomposite material, and belongs to the technical field of materials and pharmaceutical preparations. The production method comprises the following steps that: polyethylene glycol (PEG) / water is used as a solvent, and is reacted in an environment of 5 to 20 wt% of alkali solution, and the resultant product is separated by centrifugation and then washed by centrifugation, and finally, the MTX / LDHs nanocomposite material is prepared by peptization and drying. The method has theadvantages that the MTX / LDHs nancomposite material with good monodispersity can be synthesized by adding one solvent, the operation is simple, the synthetic effect is good, and no pollution to a synthetic product exists.

Description

technical field [0001] The invention belongs to the technical field of materials and pharmaceutical preparations, in particular to a co-precipitation method for preparing methotrexate / hydrotalcite-like nanocomposite materials. Background technique [0002] Hydrotalcite-like is a hydroxide with a hydrotalcite layered structure composed of two or more metal elements. The layers are positively charged and there are exchangeable anions between the layers. It is a multifunctional inorganic non-metallic material. , has a wide range of applications in catalysis, adsorption, and medicine. Its general chemical formula can be expressed as: [M 2+ 1-x m 3+ x (OH) 2 ][A n- ] x / n mH 2 O, where M 2+ Represents +2 valent metal ions, such as Mg 2+ , Zn 2+ , Mn 2+ ,Co 2+ , Ca 2+ etc.; M 3+ Indicates +3 valent metal ion, such as Cr 3+ , A1 3+ , Mn 3+ ,Co 3+ , Fe 3+ etc.; A represents interlayer anions, and different pairings of divalent and trivalent metal ions constitute a...

Claims

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Application Information

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IPC IPC(8): A61K47/48A61K47/04A61K31/519A61P35/00
Inventor 宋福贵李淑萍
Owner 江苏顺德缘文化科技股份有限公司
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