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Method for detecting dabigatran etexilate mesylate

A technology of dabigatran etexilate mesylate and a detection method, applied in the field of medicine, can solve the problem of no dabigatran etexilate mesylate and the like, and achieve a high tailing factor, good system applicability and high precision. Effect

Inactive Publication Date: 2019-11-12
JIANGXI GUOYAO PHARMA LLC
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, there is no effective detection method for dabigatran etexilate mesylate. In order to facilitate the synthesis personnel to analyze the yield, this analysis method is specially studied, which can simply, quickly and accurately determine its content

Method used

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  • Method for detecting dabigatran etexilate mesylate
  • Method for detecting dabigatran etexilate mesylate
  • Method for detecting dabigatran etexilate mesylate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] Embodiment 1: use the method for high performance liquid chromatography to detect dabigatran etexilate mesylate content

[0033] Take 1L of purified water, add 0.02mol ammonium acetate (1.54g), dissolve and add triethylamine to adjust the pH to 8.0, take 700ml of the above solution, add 1300ml of acetonitrile, mix well, and filter to obtain the mobile phase;

[0034] Take 500ml of acetonitrile, add 500ml of purified water, mix well, and prepare a diluted solution;

[0035] Take about 20mg of dabigatran etexilate mesylate, accurately weigh it, put it in a 100ml measuring bottle, add acetonitrile water (1:1) to dissolve and dilute to the mark, shake well, accurately measure 5ml and put it in a 50ml measuring bottle, add Acetonitrile water (1:1) is diluted to scale, shakes up, makes need testing solution;

[0036] Get about 20mg of dabigatran etexilate mesylate reference substance, accurately weighed, put in a 100ml measuring bottle, add acetonitrile water (1:1) to dissol...

Embodiment 2

[0039] Embodiment 2: Ammonium acetate solution and acetonitrile ratio investigation

[0040] Three mobile phases with volume ratios of 10:90, 35:65, and 70:30 were prepared using the solution containing 0.02 mol / L ammonium acetate and acetonitrile prepared according to Example 1. The rest of the conditions are the same as in Example 1, and the resolution, main peak retention time and impurity peak quantity of different mobile phases are shown in Table 1.

[0041] Table 1 The resolution, main peak retention time and impurity peak quantity of different mobile phase ratios

[0042] Ammonium Acetate: Acetonitrile Main peak retention time (min) Separation Number of impurity peaks 10:90 3.533 1.632 3 35:65 5.817 2.331 4 70:30 9.212 1.965 4

[0043] It can be seen that with the decrease of the organic phase in the mobile phase, the retention time of the main peak is extended, and the separation degree of the main peak and adjacent impurities ...

Embodiment 3

[0044] Embodiment 3: the investigation to the concentration of ammonium acetate solution

[0045] Take 1L of purified water, add 0.01mol (0.77g), 0.02mol (1.54g) and 0.03mol (2.31g) of ammonium acetate, after dissolving, add triethylamine to adjust the pH to 8.0, take 350ml of the above solution, mix it with 650ml of acetonitrile, Three mobile phases were prepared separately. All the other conditions are the same as in Example 1. The resolution, retention time of main peak and number of impurity peaks of different mobile phases are shown in Table 2.

[0046] The degree of separation and the retention time of the main peak and the number of impurity peaks of different ammonium acetate solution concentrations in table 2

[0047]

[0048] As the concentration of ammonium acetate increases, the retention time of the main peak shortens, and the resolution of the main peak and adjacent impurity peaks decreases. When the concentration is 0.02mol / L, the retention time of the main...

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Abstract

The invention relates to a method for detecting dabigatran etexilate mesylate. The method comprises the following steps: preparing a test solution and a reference solution, and then injecting the testsolution and the reference solution into a high performance liquid chromatograph for detection, wherein the test solution is prepared by dissolving a sample by using acetonitrile and water accordingto a ratio of (1 : 1), and carrying out filtering by using a microporous filter membrane; and chromatographic conditions are that octadecylsilane bonded silica is taken as a filler, a mobile phase is0.02 mol / L of ammonium acetate (the pH value is adjusted to 8.0 by triethylamine)-acetonitrile (35 : 65), a chromatographic column is the Phenomenex Gemin C18 chromatographic column with the parameters of 4.6mmX250mm and 5 microns, and the detection wavelength is 220 nm. The method disclosed by the invention has the advantages that each component obtained by analysis is good in peak shape and highin separation degree; and the method is simple to operate, high in precision, high in recovery rate and good in stability and repeatability.

Description

technical field [0001] The invention belongs to the technical field of medicines, in particular to a method for detecting the content of dabigatran etexilate mesylate. Background technique [0002] Dabigatran etexilate mesylate, developed by Boehringer Ingelheim (Boehringer Ingelheim) in Germany, was first launched in Germany and the UK in April 2008 under the trade name of Pradaxa. Dabigatran etexilate mesylate is the first new oral direct anticoagulant drug marketed in the past 50 years after warfarin. It was approved in the European Union in 2008 for the prevention of venous thrombosis after total hip or total knee replacement surgery. After oral administration, the drug releases dabigatran in the body, binds to the fibrin-specific binding site of thrombin, prevents fibrinogen from being split into fibrin, and blocks the final step of the coagulation cascade network and thrombus formation. In October 2010, FDA approved dabigatran etexilate mesylate capsules for the preve...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02G01N30/86
CPCG01N30/02G01N30/8624G01N30/8637G01N2030/047
Inventor 詹业奇万义斌葛友群左飞鸿杨明李进进艾嘉浩庄庄钟佩敏吴鑫
Owner JIANGXI GUOYAO PHARMA LLC
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