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Methylprednisolone aceponate anhydrous crystal form and composition thereof

A methylprednisolone acetonide, crystal-free technology, applied in the field of medicine, can solve the problems of high temperature and humidity requirements, increased impurities, easy water loss, etc., and achieves the effects of high safety, good dispersion state, and stable absorption

Pending Publication Date: 2020-10-09
TIANJIN PHARMA GROUP CORP
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

It has been found through research that the monohydrate crystal form, as an API, has high requirements on temperature and humidity during storage, and is prone to dehydration, and impurities will increase as the storage time of the API increases.

Method used

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  • Methylprednisolone aceponate anhydrous crystal form and composition thereof
  • Methylprednisolone aceponate anhydrous crystal form and composition thereof
  • Methylprednisolone aceponate anhydrous crystal form and composition thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] Embodiment 1 Preparation of anhydrous crystal form I of methylprednisolone acetidine

[0033] 1.1 Dissolve 10g of methylprednisolone acetate completely in 50ml of acetone, then slowly dilute it into 500ml of purified water at 0-10°C, stir for 1 hour after adding, filter to obtain methylprednisolone acetate monohydrate, and dry at 60-70°C for 14 hours. The X-ray powder diffraction measurement of the dried crystal form shows that the characteristic peak positions are 2θ=12.8°, 13.5°, 14.2°, 15.8°, 19.7°, 20.2°, such as figure 1 shown.

[0034] 1.2 Completely dissolve 10g of methylprednisolone acetidine in 40ml of methanol, then slowly dilute it into 500ml of purified water at 0-10°C, stir for 1 hour after adding, filter to obtain methylprednisolone acetate monohydrate, and dry at 70-80°C for 15 hours. The X-ray powder diffraction measurement of the dried crystal form shows that the characteristic peak positions are 2θ=12.8°, 13.5°, 14.1°, 15.8°, 19.6°, 20.1°, such as f...

Embodiment 2

[0044] The preparation of embodiment 2 acepromethylprednisolone emulsifiable cream

[0045] 2.1 Prepare 0.1% methylprednisolone acetidine cream with the crystal form I obtained in Example 1:

[0046] The prescription of methylprednisolone acetate cream is: methylprednisolone acetate 0.1g; white petrolatum 6g; stearyl alcohol 3g; glyceryl monostearate 5g; decyl oleate 5g; Pingpingjia A-201g; glycerin 5g; Disodium edetate 0.2g; benzyl alcohol 1g; polyvinylpyrrolidone 0.5g, the balance is water.

[0047] The methylprednisolone acetone crude drug is pulverized to a d(90) of 30 microns, and a d(50) of 10 microns. Precisely weigh the above ingredients, place each substance in a container, and heat until melted; then dissolve the water phase ingredients in water, mix the oil phase ingredients and water phase ingredients, heat to 85 degrees Celsius, add benzyl alcohol, and add vinegar and acrylic acid Methylprednisolone is stirred to obtain a suspension of the principal agent, and t...

Embodiment 3

[0057] The stability test of embodiment 3 bulk drug

[0058] Place the following APIs at room temperature (25±2°C) and in a colorless, transparent and closed watch glass, take samples at 1 month, 3 months, 6 months and 12 months respectively, and detect the content and related substances by HPLC: Octadecylsilane bonded silica gel is used as filler, detected by ultraviolet detector, detection wavelength is 245nm, mobile phase A is a mixed solvent of water, methanol and acetonitrile, mobile phase B is acetonitrile, gradient elution.

[0059] The results are shown in Table 1.

[0060] Table 1 API Stability Test

[0061]

[0062]

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Abstract

The invention provides a methylprednisolone aceponate anhydrous crystal form I. Characteristic peaks exist when the X-ray powder diffraction angle 2theta of the crystal form I is equal to 12.8 degrees, 14.2 degrees, 15.8 degrees, 19.7 degrees and 20.2 degrees. The preparation method of the crystal form I comprises drying methylprednisolone aceponate monohydrate to obtain the methylprednisolone aceponate crystal form I. According to the invention, the methylprednisolone aceponate in the anhydrous crystal form I is prepared as a raw material medicine, the raw material medicine of the crystal form is more stable, and after the anhydrous crystal form I of the methylprednisolone aceponate is used for preparing cream, the cream is more uniform, good in dispersion state, high in safety and stablein absorption.

Description

technical field [0001] The invention belongs to the field of medicine, and in particular relates to an anhydrous crystal form I of methylprednisolone acetidine, a preparation method thereof, and an application in cream preparations. Background technique [0002] Methylprednisolone acetate (methyprednisoloneaceponate.MPA), as the fourth-generation glucocorticoid, has the characteristics of good curative effect when used locally, good tolerance, and small systemic and local side effects. "Soft hormones". Compared with prednisolone, the introduction of the methyl group at the C6 position and the introduction of the two ester groups at the C17 and C21 positions greatly increase the lipophilicity of methylprednisolone aceprodone, and the drug molecule can quickly and effectively penetrate the stratum corneum, Effective concentrations are achieved at the treatment site. The introduction of halogen groups in the structural modification of glucocorticoids can improve the curative ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07J5/00A61K31/573A61K9/06A61P29/00A61P17/00
CPCC07J5/0053A61K9/06A61K9/0014A61K47/32A61P29/00A61P17/00C07B2200/13
Inventor 孙建磊周立飞
Owner TIANJIN PHARMA GROUP CORP
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