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High performance liquid chromatography for analyzing candesartan cilexetil

A technology of high performance liquid chromatography and candesartan cilexetil, applied in the field of medicine, can solve the problem that the actual degradation products of candesartan cilexetil are not controlled

Active Publication Date: 2011-01-05
ZHEJIANG HUAHAI PHARMA CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

"Journal of Shenyang Pharmaceutical University" No. 2, 2002, the article "Determination of Candesartan Medoxil Content by High Performance Liquid Chromatography" published by Yu Zhiguo et al., using acetonitrile-water (4:1), adjusting the pH value with phosphoric acid To 3.2 as the mobile phase, the flow rate is controlled at 1.0mL / min", both methods are to use high performance liquid chromatography isocratic elution method to determine the content of candesartan cilexetil or related substances, without or only select the The intermediate product is a known impurity, and the actual degradation products of candesartan cilexetil are not controlled

Method used

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  • High performance liquid chromatography for analyzing candesartan cilexetil
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  • High performance liquid chromatography for analyzing candesartan cilexetil

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] Instruments and Conditions:

[0031] High performance liquid chromatography: WATERS 2996, PDA detector

[0032] Chromatographic column: Agilent ZORBAX SB-C8, 4.6×100mm, 3.5μm; Buffer: Weigh 1.4g of potassium dihydrogen phosphate into 1L of water, adjust the pH to 2.2 with phosphoric acid, filter, as a buffer; mobile phase: phosphoric acid in acetonitrile Buffer; flow rate: 1.2mL / min; detection wavelength: 230nm; column temperature: 40°C; injection volume: 20μL.

[0033] Experimental steps:

[0034] (1) Take an appropriate amount of candesartan cilexetil tablet 2 mg accelerated March sample powder, dissolve it with acetonitrile: water = 3: 2 ultrasonically for 15 minutes, make a sample solution containing candesartan cilexetil 0.5 mg / mL, centrifuge, and take The supernatant was used as the sample solution.

[0035] (2) Take the above sample solution, use acetonitrile-phosphate buffer solution as the organic phase, inject 20 μL of the sample, and carry out gradient elu...

Embodiment 2

[0038] Instruments and Conditions:

[0039] High performance liquid chromatography: WATERS 2996, PDA detector

[0040] Chromatographic column: Agilent ZORBAX SB-C8, 4.6×100mm, 3.5μm; Buffer: Weigh 1.4g of ammonium dihydrogen phosphate into 1L of water, adjust the pH to 2.4 with phosphoric acid, filter, as a buffer; mobile phase: phosphoric acid in acetonitrile Buffer; flow rate: 1.0mL / min; detection wavelength: 230nm; column temperature: 30°C; injection volume: 20μL

[0041] Experimental steps:

[0042] (1) Take an appropriate amount of candesartan cilexetil tablet 2 mg accelerated March sample powder, dissolve it ultrasonically with acetonitrile: water = 3: 2, make a sample solution containing candesartan cilexetil 0.5 mg / mL, filter it, and use it as a sample solution.

[0043] (2) Take the above sample solution, use acetonitrile phosphate buffer as the organic phase, inject 20 μL of the sample, and perform gradient elution according to the following conditions. The main gra...

Embodiment 3

[0046] Instruments and Conditions:

[0047] High performance liquid chromatography: WATERS 2996, PDA detector

[0048] Chromatographic column: Agilent ZORBAX SB-C8, 4.6×100mm, 3.5μm; Buffer: Weigh 1.4g of ammonium dihydrogen phosphate into 1L of water, adjust the pH to 2.4 with phosphoric acid, filter, as a buffer; mobile phase: phosphoric acid in acetonitrile Buffer; flow rate: 1.0mL / min; detection wavelength: 230nm; column temperature: 30°C; injection volume: 20μL

[0049] Experimental steps:

[0050] (1) Alkali destruction: Take an appropriate amount of candesartan cilexetil tablet 2mg specification sample powder into a 10mL volumetric flask, add 2mL of 1N sodium hydroxide solution, leave it at room temperature for half an hour, add 1N hydrochloric acid to neutralize, dilute to volume with acetonitrile, filter, Acts as a base to destroy the sample.

[0051] (2) Acid destruction: Take an appropriate amount of candesartan cilexetil tablet 2mg sample powder into a 10mL volu...

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Abstract

The invention relates to high performance liquid chromatography for analyzing related substances of candesartan cilexetil. In the method, gradient elution is performed by adopting a reversed phase chromatographic column and taking a low-pH buffer salt of acetonitrile as a mobile phase. By the method, all known impurities of the candesartan cilexetil can be simultaneously analyzed, the problems that unknown impurities interfere with the candesartan cilexetil in the prior art and the degradation product of the candesartan cilexetil cannot be controlled by a conventional liquid phase analytic method are solved, and the quality of raw materials or preparation of the candesartan cilexetil can be more comprehensively and effectively controlled. The method has the advantages of simple operation,high repeatability and higher specificity.

Description

technical field [0001] The invention relates to the determination of related substances of candesartan cilexetil by high performance liquid chromatography. The method better controls the impurities in candesartan cilexetil raw materials and preparations, and provides guarantee for patients' healthy drug use. It belongs to medical technology field. Background technique [0002] Candesartan cilexetil, the chemical name is 2-ethoxy-1-[[2'-(1H-tetrazol-5-yl)[1,1'-biphenyl]-4-yl]methyl ]-1H-benzimidazole-7-carboxylic acid-1-[[(cyclohexyloxy)carbonyl]oxy]ethyl ester, which has a small dose (much smaller than other sartan drugs), significant antihypertensive effect, It has the advantages of reversing the hypertrophy of the heart wall, preventing myocardial infarction, less side effects, good tolerance, and has a protective effect on renal failure. Candesartan cilexetil is unstable, especially the impurities in the preparation grow rapidly, there are many degradation products and ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02
Inventor 代军张伦杨长青王红莲
Owner ZHEJIANG HUAHAI PHARMA CO LTD
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