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Preparation method for methotrexate/layered double hydroxide nanocomposite

A nano-composite material, layered bimetal technology, applied in the direction of drug combination, medical preparations with non-active ingredients, medical preparations containing active ingredients, etc. resources and other issues, to achieve the effect of low equipment cost, energy saving and pollution reduction

Inactive Publication Date: 2013-05-15
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

[0004] At present, the methods for preparing MTX / LDHs include high-temperature solid-phase method, co-precipitation method and ion exchange method. It is carried out in aqueous solution, which takes a long time, wastes water resources and pollutes the environment
This has a certain impact on the application and industrial production of MTX / LDHs, which does not meet the current theme of "environmental protection and green"

Method used

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  • Preparation method for methotrexate/layered double hydroxide nanocomposite
  • Preparation method for methotrexate/layered double hydroxide nanocomposite
  • Preparation method for methotrexate/layered double hydroxide nanocomposite

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] 1) At room temperature, Mg(NO 3 ) 2 ?6H 2 O and Al(NO 3 ) 3 ?9H 2 O carry out pre-grinding 2min;

[0034] 2) Prepare a NaOH solution with a concentration of 10.5mol / L;

[0035] 3) Weigh 0.7692g Mg(NO 3 ) 2 ?6H 2 O and 0.5627g Al(NO 3 ) 3 ?9H 2 O placed in an agate mortar in which Mg 2+ / Al 3+ =2:1; add 0.3408g MTX, then drop 1.15ml of the NaOH solution prepared in step 2), mix well, and grind at a constant speed for 60min. Centrifuged and washed 4 times with distilled water to obtain the MTX / LDH precursor;

[0036] 4) Add water to the precursor prepared in step 3) and sonicate to prepare a 2mol / L precursor solution, and then put it into a polytetrafluoroethylene-lined reactor for peptization. The peptization temperature is 80°C. The melting time was 24 hours, and the product was dried to obtain the MTX / LDH nanocomposite material.

[0037] figure 1 The XRD pattern of the MTX / LDH nanocomposite material that is the present embodiment made, figure 1 showed...

Embodiment 2

[0041] 1) At room temperature, Zn(NO 3 ) 2 ?6H 2 O and Al(NO 3 ) 3 ?9H 2 O carries out pre-grinding 5min;

[0042] 2) Prepare NH with a concentration of 8mol / L 3 ?H 2 O solution;

[0043] 3) Weigh 0.9520g Zn(NO 3 ) 2 ?6H 2 O and 0.5627g Al(NO 3 ) 3 ?9H 2 O is placed in a grinding tool, where Zn 2+ / Al 3+ =2:0.8; add 0.3636 gMTX, then drop 2.8ml of NH prepared in step 2) 3 ?H 2 O solution, mix evenly, and grind at a constant speed for 40 minutes. Centrifuged and washed 3 times with distilled water to obtain the MTX / LDH precursor;

[0044] 4) Add water to the precursor prepared in step 3) and sonicate to prepare a 0.5mol / L precursor solution, put it in the reaction kettle for peptization, the peptization temperature is 100°C, and the peptization time is 48h, and the product is dried. Prepared MTX / LDH nanocomposites.

[0045] The resulting XRD pattern shows that: with the parent LDH-NO 3 Compared to the composite d 003 The characteristic diffraction peak shi...

Embodiment 3

[0047] 1) At room temperature, Mg(NO 3 ) 2 ?6H 2 O and Fe(NO 3 ) 3 ?9H 2 O carries out pre-grinding 3min;

[0048] 2) Prepare a NaOH solution with a concentration of 12mol / L;

[0049] 3) Weigh 0.6410 g Mg(NO 3 ) 2 ?6H 2 O and 0.6060g Fe(NO 3 ) 3 ?9H 2 O placed in the grinding utensils, wherein, Mg 2+ / Fe 3+ =2:1.2; Add 0.2840 gMTX, then drop 1.57ml of the NaOH solution prepared in step 2), mix well, and grind at a constant speed for 160min. Centrifuged and washed 4 times with distilled water to obtain the MTX / LDH precursor;

[0050] 4) Add water to the precursor prepared in step 3) and sonicate it to prepare a 3mol / L precursor solution, and put it into a polytetrafluoroethylene-lined reactor for peptization. The peptization temperature is 120°C. The time was 12 h, and the product was dried to obtain the MTX / LDH nanocomposite material.

[0051] The resulting XRD pattern shows that: with the parent LDH-NO 3 Compared to the composite d 003 The characteristic dif...

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Abstract

The invention discloses a preparation method for methotrexate / layered double hydroxide (MTX / LDHs) nanocomposite, which belongs to the technical fields of the material and the pharmaceutical preparation. The preparation method comprises the following steps of: 1) respectively pre-grinding bivalent metal salt and trivalent metal salt; 2) preparing aqueous alkali of which the concentration is 8-12mol / L; 3) respectively weighing the bivalent metal salt and the trivalent metal salt obtained in step 1), putting the bivalent metal salt and the trivalent metal salt into a mortar, and adding the methotrexate (MTX); dripping aqueous alkali obtained in step 2), evenly mixing the above substances, grinding for a certain time at constant speed, and carrying out centrifugal washing to mixture by distilled water to obtain an MTX / LDH precursor; and 4) dispersing the MTX / LDH precursor into water, putting into a reaction kettle for peptization, and drying an obtained peptized product. By adopting the mechanochemistry method, a product with regular particle morphology and good monodispersity is prepared, and the preparation method is environmentally friendly.

Description

technical field [0001] The invention belongs to the technical field of materials and pharmaceutical preparations, and in particular relates to a method for preparing a methotrexate / layered double metal hydroxide nanocomposite material. Background technique [0002] Layered double hydroxides (LDHs for short), also known as hydrotalcite like compounds (HTlc for short), the general chemical formula can be expressed as: [M 2+ 1-x m 3+ x (OH) 2 ] x+ [A n- ] x / n mH 2 O, where M 2+ Indicates a divalent metal ion, M 3+ means trivalent metal ion, x means M 2+ / (M 2+ +M 3+ ) molar ratio, A represents the interlayer anion, m is the number of crystal water. The structure of such materials consists of positively charged brucite-like layers [M 2+ (OH) 2 ] and interlayer exchangeable anions and water molecules. LDHs have a unique laminate structure, which can effectively protect the molecules or ions inserted into it. By changing the types of metal cations and interlayer an...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): A61K47/48A61K31/519A61P35/00A61P35/02A61P19/02A61P29/00A61P17/06
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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