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High performance liquid chromatography analysis method of azilsartan medoxomil

A technology of high-performance liquid chromatography and analysis method, which is applied in the field of high-performance liquid chromatography analysis of related substances in azilsartan raw materials and its preparations, can solve the problems of no literature reports, etc., and achieve the effect of strong specificity

Active Publication Date: 2014-04-23
HEFEI JIUNUO MEDICAL TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] Azilsartan raw material and its preparation related substances analysis method has not been reported in the literature

Method used

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  • High performance liquid chromatography analysis method of azilsartan medoxomil
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  • High performance liquid chromatography analysis method of azilsartan medoxomil

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0045] Detection equipment and chromatographic conditions:

[0046] High performance liquid chromatography: SSI Series1500PUMP, Series1500PDA detector

[0047] Chromatographic column: Agilent C18 (250×4.6mm, 5μm); mobile phase A: acetonitrile-low-concentration acetic acid aqueous solution with a volume ratio of 57:43, wherein the volume ratio of water to acetic acid in the low-concentration acetic acid aqueous solution is 43:1 Mobile phase B: acetonitrile-low-concentration acetic acid aqueous solution with a volume ratio of 90:10, wherein the volume ratio of water and acetic acid in the low-concentration acetic acid aqueous solution is 10:1; flow rate: 0.8ml / min; detection wavelength: 250nm; Column temperature: 30°C; injection volume: 10 μl.

[0048] Experimental steps:

[0049] (1) Sample preparation:

[0050] Take an appropriate amount of azilsartan and known impurities A~J, add acetonitrile-water (volume ratio 3:2) to ultrasonically dissolve and dilute to make about 0.4 mg...

Embodiment 2

[0055] Detection equipment and chromatographic conditions:

[0056] High performance liquid chromatography: SSI Series1500PUMP, Series1500PDA detector

[0057] Chromatographic column: Agilent C18 (250×4.6mm, 5μm); mobile phase A: same as Example 1, mobile phase B: same as Example 1; flow rate: 0.8ml / min; detection wavelength: 250nm; column temperature: 30°C; Injection volume: 10 μl.

[0058] Experimental steps:

[0059] (1) Sample preparation:

[0060] Acid destruction: take azilsartan tablet, grind it finely, take an appropriate amount of fine powder (about 20mg containing azilsartan), put it in a 50ml brown measuring bottle, add 5ml of 1mol / L hydrochloric acid solution, shake well, and place in a 60°C water bath Heating for 2 hours, after cooling, add 5ml of 1mol / L sodium hydroxide solution to neutralize, then dilute to the mark with acetonitrile-water solution (the same below) with a volume ratio of 3:2, shake well, filter, and use it as an acid-damaged sample;

[0061]...

Embodiment 3

[0069] Detection equipment and chromatographic conditions:

[0070] High performance liquid chromatography: SSI Series1500PUMP, Series1500PDA detector

[0071] Chromatographic column: Agilent C18 (250×4.6mm, 5μm); mobile phase A: same as Example 1, mobile phase B: same as Example 1; flow rate: 0.8ml / min; detection wavelength: 254nm; column temperature: 30°C; Injection volume: 10μl

[0072] Experimental steps:

[0073] (1) Sample preparation: take azilsartan tablet (20mg), grind it into fine powder, take an appropriate amount of fine powder (approximately equivalent to 20mg containing azilsartan), dissolve and dilute with acetonitrile-water (volume ratio 3:2) ultrasonically Prepare a solution containing 0.4 mg / ml of azilsartan as a sample solution

[0074] (2) Gradient elution program setting: same as in Example 1.

[0075] (3) Detection: Take the above sample solution, inject 10 μl, and record the chromatogram.

[0076] See attached for typical chromatogram Figure 7 . ...

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Abstract

The invention discloses a high performance liquid chromatography analysis method of azilsartan medoxomil. The method employs a reversed phase chromatography column and an ultraviolet detector, and an aqueous solution containing acetonitrile and acetic acid of low concentration is used as a mobile phase for gradient elution. The method can be used for simultaneously analyzing azilsartan medoxomil raw materials and all impurities in the preparation, and content of each known impurity can be effectively controlled by using a principle component self-contrasted method with correction factor added, and resolutions between each impurity peak, and resolutions between the main peak and adjacent impurity peaks are higher than 1.5, and purities of the main peak and each impurity peak are 1.0. The analysis method is simple with good repeatability and high specialization.

Description

1. Technical field [0001] The invention relates to a method for analyzing the purity of chemical medicines, in particular to a high performance liquid chromatography analysis method for related substances in azilsartan raw materials and its preparations. 2. Background technology [0002] Azilsartan (azilsartan), chemical name 2-ethoxy-1-[[2'-(4,5-dihydro-5-oxo-1,2,4-oxadiazol-3-yl ) biphenyl-4-yl] methyl]-1H-benzimidazole-7-carboxylic acid, the chemical structural formula is the following formula (I): [0003] [0004] Azilsartan is an angiotensin II receptor antagonist developed by Takeda Corporation of Japan and launched in Japan in May 2012. The clinical results show that taking azilsartan at 20mg / d and 40mg / d, the 24h average ambulatory blood pressure and systolic blood pressure decrease significantly better than that of olmesartan medoxomil and valsartan, and azilsartan can also partially activate peroxidation. Proteosomal proliferators activate receptor-γ and have...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02
Inventor 吴标崔红晓王娟汪电雷
Owner HEFEI JIUNUO MEDICAL TECH
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