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 inactive ingredients, medical preparations containing active ingredients, etc. Large and other problems, to achieve the effect of low equipment cost, energy saving and pollution reduction

Inactive Publication Date: 2012-08-22
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,

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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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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