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Method for detecting methylprednisolone aceponate content and related substances

A technology of methylprednisolone acetate and related substances, which is applied in the detection field of methylprednisolone acetate and related substances, and can solve problems such as instability, inability to achieve effective separation, and late peaking

Pending Publication Date: 2020-07-07
TIANJIN PHARMA GROUP CORP
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In view of the detection of process impurities and degradation impurities contained in methylprednisolone acetate, the structure is relatively similar, and the conventional buffer salt system and the mobile phase containing acid and alkali cannot achieve effective separation
Moreover, the polarity of MPA-ZZ5 and MPA-ZZ6 among the above impurities is relatively small, and the peak is relatively late
[0007] The 2014 document "Quality Research and Stability Investigation of Methylprednisolone Acetate Raw Materials" discloses the quality standards for detecting methylprednisolone acetate and the detection method of related substances, but in this method, the sample solution is methanol: acetonitrile: Water is 40:5:55, acepromethylprednisolone is the structure containing ester, encounters protic solvent easily unstable, as methanol, water, easily causes the hydrolysis of sample; The mobile phase A used in this method is sample solution; Mobile phase B is methanol, using gradient elution
[0009] It has been verified that the methods for the determination of methylprednisolone acetate in the above documents cannot completely separate the above impurities

Method used

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  • Method for detecting methylprednisolone aceponate content and related substances
  • Method for detecting methylprednisolone aceponate content and related substances
  • Method for detecting methylprednisolone aceponate content and related substances

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0039] System suitability solution: Accurately weigh methylprednisolone acetate reference substance to prepare about 1.0 mg / ml of methylprednisolone acetate; take MPA-ZZ1 reference substance, MPA-ZZ2 reference substance, MPA-ZZ3 reference substance, MPA - ZZ4 reference substance, MPA-ZZ5 reference substance, MPA-ZZ6 reference substance, MPA-ZZ8 reference substance, MPA-ZZ9 reference substance and MPA-ZZ7 reference substance are prepared in appropriate amounts to contain 20.0 μg / ml, and mixed to obtain system suitability solution.

[0040] Blank solution: use acetonitrile as the blank solution.

[0041] Determine according to high-performance liquid chromatography (Chinese Pharmacopoeia 2015 edition four general rules 0512). Use octadecylsilane bonded silica gel as filler (250mm×4.6mm, 5μm) chromatographic column; use water-methanol-acetonitrile (40:40:20) as mobile phase A and acetonitrile as mobile phase B, press Gradient elution is carried out; the detection wavelength is ...

Embodiment 2

[0047] Need testing solution: take the appropriate amount of methylprednisolone acetate of MPA0810 batch, accurately weighed, add acetonitrile to dissolve and quantitatively dilute to make a solution containing about 1.0mg in every 1ml, as the need testing solution.

[0048] Reference substance solution: take 1ml of the test solution and put it in a 100ml measuring bottle, add acetonitrile to dilute to the mark, shake well, then accurately measure 1ml, put it in a 10ml measuring bottle, add acetonitrile to dilute to the mark, shake well, and use as Control solution.

[0049] Blank solution: use acetonitrile as the blank solution.

[0050] According to the following experimental conditions, take 20 μl each of the blank solution, the test solution and the reference solution, inject them into the liquid chromatograph respectively, adjust the detection sensitivity, and record the chromatograms. The chromatographic conditions are as follows:

[0051] Use octadecylsilane bonded si...

Embodiment 3

[0057] System suitability solution: Accurately weigh methylprednisolone acetate reference substance to prepare about 1.0 mg / ml of methylprednisolone acetate; take MPA-ZZ1 reference substance, MPA-ZZ2 reference substance, MPA-ZZ3 reference substance, MPA - ZZ4 reference substance, MPA-ZZ5 reference substance, MPA-ZZ6 reference substance, MPA-ZZ8 reference substance, MPA-ZZ9 reference substance and MPA-ZZ7 reference substance are prepared in appropriate amounts to contain 20.0 μg / ml, and mixed to obtain system suitability solution.

[0058] Blank solution: use acetonitrile as the blank solution.

[0059] Determine according to high-performance liquid chromatography (Chinese Pharmacopoeia 2015 edition four general rules 0512). Use octadecylsilane bonded silica gel as filler (250mm×4.6mm, 5μm) chromatographic column; use water-methanol-acetonitrile (40:40:20) as mobile phase A and acetonitrile as mobile phase B, press Gradient elution is carried out; the detection wavelength is ...

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Abstract

The invention provides a method for detecting the methylprednisolone aceponate content and related substances. Column chromatography is employed, octadecylsilane chemically bonded silica is used as afiller, an ultraviolet detector is used for detecting, the detection wavelength is 235-255 nm, the mobile phase A is a mixed solvent of water, methanol and acetonitrile, wherein the ratio of water is38%-42%, the ratio of methanol is 38%-42%, the ratio of acetonitrile is 16%-24%, and the mobile phase B is acetonitrile, and gradient elution is performed. The method has the beneficial effects that the content of methylprednisolone aceponate and nine contained related substances can be accurately and effectively detected and separated at the same time, and the method has good specificity and accuracy and is suitable for detecting the content of methylprednisolone aceponate and the related substances.

Description

technical field [0001] The invention belongs to the field of drug analysis, in particular to a method for detecting the content of methylprednisolone acetidine and related substances. Background technique [0002] As a fourth-generation glucocorticoid, methylprednisolone acetone has the characteristics of good curative effect when used locally, good tolerance, and small systemic and local side effects. It belongs to the "soft hormone" that has been highly praised by scholars from all over the world in recent years. 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 t...

Claims

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Application Information

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IPC IPC(8): G01N30/02G01N30/74G01N30/34
CPCG01N30/02G01N30/74G01N30/34
Inventor 贾美娜刘晓明郭志强
Owner TIANJIN PHARMA GROUP CORP
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