Method for determining impurities in candesartan cilexetil

A technology for candesartan medoxomil and impurities, which is applied in the field of food and drug safety testing, can solve the problems of insufficient pertinence of impurity control, poor accuracy, and difficulty in popularizing detection methods, and achieves long purchasing cycle, strong pertinence and good quality. The effect of applying value

Active Publication Date: 2020-07-28
广东省药品检验所
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Therefore, it is urgent to find a convenient method for detecting impurities in candesartan cilexetil, so as to improve the current situation that the impurity control in the quality standard of candesartan cilexetil is not targeted enough, the accuracy is not strong, or the detection method is difficult to popularize, so as to ensure Candesartan cilexetil solution containing impurities A, B, C, D, E, F, G can be easily obtained in the daily inspection process, which is used for the positioning of related substances in the analysis of this variety

Method used

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  • Method for determining impurities in candesartan cilexetil
  • Method for determining impurities in candesartan cilexetil
  • Method for determining impurities in candesartan cilexetil

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Embodiment 1

[0051]The determination of impurity in embodiment 1 candesartan cilexetil

[0052] The structural formula of impurities (impurity A, B, C, D, E, F or G) in candesartan cilexetil and candesartan cilexetil is shown in Table 1, wherein, impurity A is a synthetic by-product, impurity B, C, D, E, and F are impurities, and impurity G is a synthetic starting material, which will be degraded to varying degrees under various damage conditions; according to the structural characteristics of the product, impurities B, C, D, E, and F are candi The main degradation impurity of sartan cilexetil.

[0053] Table 1 candesartan cilexetil and the structural formula of impurities in candesartan cilexetil

[0054]

[0055]

[0056] Through the destruction experiment, adopting candesartan cilexetil standard substance can destroy impurity A, B, C, D, E, F, G, through repeated experimentation, adopt the measurement of impurity in the candesartan cilexetil provided by this embodiment 1 Methods...

Embodiment 2

[0080] The determination of impurity in embodiment 2 candesartan cilexetil

[0081] 1. Experimental method

[0082] A method for measuring impurities in candesartan cilexetil, comprising the following steps:

[0083] S1. Take 20mg of candesartan cilexetil standard product, put it in a graduated test tube, add 50mL of acetonitrile-water (volume ratio 3:2) mixed solution to dissolve, shake well, heat in a water bath (100°C) for 1.5h, take it out, and let it cool until At room temperature, add acetonitrile (50% by volume) to 50 mL, shake well to obtain degradation solution 1;

[0084] In addition, take 20 mg of candesartan cilexetil standard product, put it in a 50 mL volumetric flask, dissolve it with ethanol, add 25 mL of 0.5 mol / L calcium hydroxide solution, let it stand for 15 min, add 2.5 mL of 0.5 mol / L sulfuric acid for neutralization, and then dissolve it with ethanol Constant volume to obtain degradation solution 2; take degradation solution 1 and degradation solution ...

Embodiment 3

[0093] The determination of impurity in embodiment 3 candesartan cilexetil

[0094] 1. Experimental method

[0095] A method for measuring impurities in candesartan cilexetil, comprising the following steps:

[0096] S1. Take 40 mg of candesartan cilexetil standard (purchased from China National Institutes for Food and Drug Control), put it in a graduated test tube, add 100 mL of acetonitrile-water (volume ratio 3:2) mixed solution to dissolve, shake well, and heat in a water bath (100 ℃) for 3 hours, take it out, let it cool to room temperature, add acetonitrile (50% by volume) to 100mL, shake well, and obtain degradation solution 1;

[0097]In addition, take 10 mg of candesartan cilexetil standard product, put it in a 25 mL volumetric flask, dissolve it with ethanol, add 25 mL of 0.5 mol / L potassium hydroxide solution, let it stand for 15 min, add 2.5 mL of 0.5 mol / L nitric acid for neutralization, and then dissolve it with ethanol Constant volume to obtain degradation sol...

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Abstract

The invention discloses a method for determining impurities in candesartan cilexetil. The method comprises the following steps: S1, heating a candesartan cilexetil standard substance solution at 70-100 DEG C for 1.5-3 hours, cooling, and adding acetonitrile to obtain a degradation solution 1; besides, adding the candesartan cilexetil standard substance solution into an alkaline solution, performing standing for 5-30 minutes, and adding an acid solution for neutralization to obtain a degradation solution 2; mixing the degradation solution 1 and the degradation solution 2 to obtain a system applicability solution; S2, dissolving candesartan cilexetil to be detected, and quantitatively preparing a test solution; diluting the test solution as a control solution; and S3, respectively carrying out liquid chromatography detection on the system suitability solution obtained in the step S1, the test solution obtained in the step S2 and the control solution, and determining the impurities A, B,C, D, E, F or G in candesartan cilexetil by comparing liquid chromatograms. The method is strong in pertinence, high in accuracy and easy to popularize, and has good application value in the aspect ofdetermining the impurities in candesartan cilexetil.

Description

technical field [0001] The invention belongs to the technical field of food and drug safety detection. More specifically, it relates to a method for determining impurities in candesartan cilexetil. Background technique [0002] Candesartan cilexetil is a prodrug that is rapidly and completely converted to the active metabolite candesartan during absorption. Candesartan is a selective angiotensin II type 1 receptor (AT1) antagonist of diphenyltetramisole, which acts on the renin-angiotensin-aldosterone system and has an inhibitory effect on angiotensin II type 1 receptor (AT1). It has strong affinity and is produced both at home and abroad. It is clinically used to treat diseases such as hypertension, atherosclerosis, congestive heart failure, and myocardial infarction. [0003] At present, the control methods of impurities (impurities A, B, C, D, E, F, G) in candesartan cilexetil are in the Chinese Pharmacopoeia 2015 edition, BP2019 (raw material / tablet) and USP42-NF37 (ta...

Claims

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Application Information

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IPC IPC(8): G01N30/06G01N30/86
CPCG01N30/06G01N30/8634
Inventor 余少文王彩媚吴纯敏
Owner 广东省药品检验所
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