High performance liquid chromatography analyzing method of eplerenone related substances

A technology of high-performance liquid chromatography and analysis method, which is applied in the direction of analyzing materials, material separation, measuring devices, etc., can solve the problems that are not conducive to production control, have no literature reports, and do not clearly detect the impurity spectrum and impurity structure, and achieve great positive results. Progressive effect and practical application value, the effect of strong method specificity

Active Publication Date: 2016-08-17
HEFEI JIUNUO MEDICAL TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Patent CN200610096055.2 discloses a method for detecting impurities in eplerenone raw materials or its preparations. This method does not locate known impurities. Experiments have proved that this method cannot effectively detect and separate the above-mentioned known impurities; patent CN200810246556. 3 discloses a method for determining the cis-trans isomers of eplerenone, but also does not clearly detect the impurity profile and impurity structure, which is not conducive to production control
[0008] Based on comprehensive impurity profile analysis, there is no relevant literature report on the analysis method of related substances in eplerenone raw materials and its preparations

Method used

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  • High performance liquid chromatography analyzing method of eplerenone related substances
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  • High performance liquid chromatography analyzing method of eplerenone related substances

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Experimental program
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Effect test

Embodiment 1

[0041] Detection equipment and chromatographic conditions:

[0042] High performance liquid chromatography: SSI Series 1500PUMP, Series 1500DAD detector

[0043] Chromatographic column: Hypersil C18 (150×4.6mm, 5μm); mobile phase: acetonitrile-methanol-0.01mol / L phosphate buffer with a volume ratio of 10:35:55 ​​(adjust the pH value to 3.0 with phosphoric acid); detection wavelength : 243nm; flow rate: 1.0ml / min; column temperature: 30°C; injection volume: 20μl.

[0044] Experimental steps:

[0045] (1) Sample preparation:

[0046] Take an appropriate amount of eplerenone and known impurities A-J, ultrasonically dissolve and dilute with a mixed solution of acetonitrile and water with a volume ratio of 3:2 to make eplerenone about 0.5 mg / ml and impurities A-G about 5 μg / ml. ml and impurity H-J are about 50μg / ml solution, as the sample solution.

[0047] (2) Detection: Take the above sample solution, inject 20 μl of it, and record the chromatogram.

[0048] For a typical ch...

Embodiment 2

[0050] Detection equipment and chromatographic conditions:

[0051] High performance liquid chromatography: SSI Series 1500PUMP, Series 1500DAD detector

[0052] Chromatographic column: Hypersil C18 (150×4.6mm, 5μm); mobile phase: acetonitrile-methanol-0.01mol / L phosphate buffer with a volume ratio of 10:35:55 ​​(adjust the pH value to 3.0 with phosphoric acid); detection wavelength : 243nm; flow rate: 1.0ml / min; column temperature: 30°C; injection volume: 20μl.

[0053] (1) Sample preparation:

[0054] Acid destruction: Take eplerenone tablet, grind it finely, take an appropriate amount of fine powder (about 25mg containing eplerenone), put it in a 50ml measuring bottle, add 10ml of 1mol / L hydrochloric acid solution, shake well, and heat in a water bath for 15 minutes , after cooling, add 10ml of 1mol / L sodium hydroxide solution for neutralization, then ultrasonically treat the mixed solution of acetonitrile and water with a volume ratio of 3:2 to dissolve eplerenone and di...

Embodiment 3

[0063] Detection equipment and chromatographic conditions:

[0064] High performance liquid chromatography: SSI Series 1500PUMP, Series 1500DAD detector

[0065] Chromatographic column: Hypersil C18 (150×4.6mm, 5 μm); mobile phase: acetonitrile-methanol-0.01mol / L phosphate buffer with a volume ratio of 10:35:55 ​​(adjust the pH value to 3.0 with phosphoric acid); detection wavelength : 243nm; flow rate: 1.0ml / min; column temperature: 30°C; injection volume: 20μl.

[0066] Experimental steps:

[0067] (1) Sample preparation: Take an appropriate amount of eplerenone, and use an appropriate amount of acetonitrile and water mixed solution with a volume ratio of 3:2 to sonicate to dissolve and dilute to make a solution containing about 0.5 mg per 1 ml, shake well, and use it as a sample solution.

[0068] (2) Detection: Take the above sample solution, inject 20 μl of it, and record the chromatogram.

[0069] For a typical chromatogram see Figure 8 .

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Abstract

The invention discloses a high performance liquid chromatography analyzing method of eplerenone related substances. The high performance liquid chromatography analyzing method is characterized in that a reversed-phase chromatographic column and an ultraviolet detector are used and an acetonitrile-methanol-phosphate buffer solution is used as the flowing phase to perform isocratic elution. The high performance liquid chromatography analyzing method has the advantages that all the known impurities in eplerenone raw materials and eplerenone preparations can be analyzed at the same time, the content of the known impurities can be effectively controlled through the self-contrasted method of the main component added with correction factors, the separation degree between a main peak and an impurity peak adjacent to the main peak and between every two impurity peaks is larger than 1.5, and the purity of the main peak and the impurity peaks is 1.0. By the high performance liquid chromatography analyzing method, a simple and reliable analyzing method is provided for the quality control analyzing of the eplerenone raw materials and the eplerenone preparations.

Description

1. Technical field [0001] The invention relates to an analysis method for the purity of chemical drugs, in particular to a high-performance liquid chromatography analysis method for eplerenone related substances. 2. Background technology [0002] Eplerenone, chemical name 9α, 11α-epoxy-17β-hydroxy-3-oxo-17α-pregna-4-ene-7α, 21-dicarboxylic acid, γ-lactone, 7 - methyl ester, the chemical structural formula is as follows: [0003] [0004] Eplerenone (Eplerenone) is a new generation of selective aldosterone antagonist developed by Pfizer / Pharmacia, and its trade name is It was first launched in the United States in September 2002, and it is currently listed in the United Kingdom, France, Japan, Germany, etc., for the treatment of hypertension, heart failure and myocardial infarction. It has definite curative effect on the treatment of hypertension, heart failure and myocardial infarction, with less adverse reactions and good tolerance. Its outstanding advantage is that ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02
CPCG01N30/02G01N2030/027
Inventor 吴标王娟施伶俐崔红晓
Owner HEFEI JIUNUO MEDICAL TECH
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