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A kind of detection method of genotoxic impurity of candesartan cilexetil

A technology for candesartan cilexetil and genotoxicity, which is applied in the field of analysis of the genotoxic impurity 1-chloroethylcyclohexyl carbonate of candesartan cilexetil, and can solve the detection of interfering impurity 1-chloroethylcyclohexyl carbonate , high price, restrictions on the promotion of the method, etc., to achieve the effect of low detection cost, accurate and feasible method, and easy promotion

Active Publication Date: 2021-08-13
迪嘉药业集团股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0010] Literature "Method development and validation by GC-MS for quantification of 1-chloroethyl cyclohexyl carbonate as a genotoxic impurity in candesartancilexetil drug substance" (Nalavade Atul Kakasaheb, Ramakrishna K, Srinivasarao V. Method Development and Validation by Qu-Ch-MS for GC-ro Cyclohexyl Caronate as a Genotoxic Impurity in Candesartan Cilexetil Drug Substance. International Journal of Pharmacy and Pharmaceutical Sciences.2014, vol6, Issue11:370-372) uses GC-MS to detect impurity 1-chloroethyl cyclohexyl carbonate, and the literature uses acetone as solvent , there are the following defects: one is that candesartan cilexetil is insoluble in acetone; the other is that candesartan cilexetil will degrade under high temperature conditions above 170°C, and the degraded substances will enter the mass spectrometer detector, and repeated injections will interfere with impurities 1- Chloroethylcyclohexyl carbonate detection, and contamination of the detector, resulting in inaccurate detection results
And the use of gas phase-mass spectrometry detector is expensive, which limits the promotion of the method

Method used

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  • A kind of detection method of genotoxic impurity of candesartan cilexetil
  • A kind of detection method of genotoxic impurity of candesartan cilexetil
  • A kind of detection method of genotoxic impurity of candesartan cilexetil

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specific Embodiment approach

[0063] DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS The present invention will be further described below in conjunction with specific examples. It should be understood that these examples are only used to illustrate the present invention and are not intended to limit the protection scope of the present invention. Embodiments of the present invention are described below through specific examples, and those skilled in the art can easily understand other advantages and effects of the present invention from the content disclosed in this specification. The present invention can also be implemented or applied through other different specific implementation modes, and various modifications or changes can be made to the details in this specification based on different viewpoints and applications without departing from the spirit of the present invention.

[0064] The reagents and instruments used in the following examples are as follows:

[0065] Reagent:

[0066] Acetonitrile:...

Embodiment 1

[0077] Example 1 Optimization of reaction vessel and dosage of candesartan cilexetil.

[0078] Experimental part:

[0079] 1.1 Sample pretreatment:

[0080] (1) 100ml eggplant-shaped bottle as reaction vessel:

[0081] The test product (sampling) solution: Weigh about 5g of candesartan cilexetil, about 1g of potassium carbonate and about 0.1g of potassium iodide, and put them in the same 100ml eggplant-shaped reaction bottle; accurately measure the impurity 1-chloroethylcyclohexyl carbonate Add 5ml of ester stock solution (49.30μg / ml) into the bottle, then add 5ml of N,N-dimethylformamide, shake well, put it in a magnetic rotor, put it in a water bath at 60°C and stir and heat for 6h, then filter the reaction solution with filter paper Filter into a 100ml measuring bottle, then rinse the reaction bottle with acetonitrile, and filter the rinse solution into the same measuring bottle, dilute to volume with acetonitrile, and shake well; then accurately measure 5ml, place it in ...

Embodiment 2

[0094] The investigation of embodiment 2 derivatization temperature

[0095] 1. Experimental part

[0096] 1.1 Sample pretreatment

[0097] The test product (sampling) solution: weigh about 2g of candesartan cilexetil, about 0.5g of potassium carbonate and about 0.05g of potassium iodide, and put them in the same 25ml eggplant-shaped reaction bottle; accurately measure the impurity 1-chloroethylcyclohexyl Add 2ml of carbonate stock solution (51.33μg / ml) into the bottle, then add 2ml of N,N-dimethylformamide, shake well, and put it into the magnetic rotor. Prepare 3 parts of the test solution according to the above preparation method, place them in water baths at 40°C, 50°C, and 60°C respectively, stir and heat for 5 hours, then filter the reaction solution into a 100ml measuring bottle with filter paper, then rinse the reaction bottle with acetonitrile, and Filter the rinse solution and put it in the same measuring bottle, dilute it with acetonitrile, and shake it well; then...

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Abstract

The invention relates to a method for analyzing the genotoxic impurity 1-chloroethylcyclohexyl carbonate of candesartan cilexetil, belonging to the technical field of crude drug analysis. The present invention utilizes the impurity 1-chloroethyl cyclohexyl carbonate existing in candesartan cilexetil and the pre-column derivation method of the derivation reaction with candesartan cilexetil itself to measure the impurity 1-chloroethyl cyclohexyl carbonate content, to achieve the control of genotoxic impurity 1-chloroethyl cyclohexyl carbonate in candesartan cilexetil. The invention provides a detection method for the genotoxic impurity in candesartan cilexetil, which provides guarantee for the quality control of candesartan cilexetil preparations.

Description

technical field [0001] The invention relates to a method for analyzing the genotoxic impurity 1-chloroethylcyclohexyl carbonate of candesartan cilexetil, belonging to the technical field of raw material medicine quality control. Background technique [0002] Genotoxic impurities are closely related to the quality and safety of drugs. The existence of genotoxic impurities may cause toxic and side effects to the human body, and even cause gene mutations or cancer. Therefore, it is necessary to control the type and content of genotoxic impurities in the drug through appropriate detection and analysis methods to ensure the quality of the drug. [0003] Candesartan cilexetil is a selective angiotensin II receptor (ATI) antagonist indicated for essential hypertension with the chemical name (±)-l-[(cyclohexyloxy)carbonyloxy] Ethyl 2-ethoxy-1 -[ [2'-(1 H -tetrazolyl-5-yl)biphenyl-4-yl]methyl]-1 H -benzimidazole-7-carboxylate, the chemical structural formula is as follows: [000...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/88G01N30/06
CPCG01N30/06G01N30/88G01N2030/047
Inventor 刘敏李晶高钦磊
Owner 迪嘉药业集团股份有限公司
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