Method for detecting related substances or/and content thereof for dabigatran etexilate mesylate and dabigatran etexilate mesylate preparations

A technology for dabigatran etexilate mesylate and related substances, which is applied in the field of detection of dabigatran etexilate mesylate or its preparation related substances or/and contents, can solve problems such as inability to detect impurities of related substances, and achieves the The effect of good chromatographic peak resolution

Active Publication Date: 2019-07-05
CHENGDU BRILLIANT PHARMA CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The technical problem mainly solved by the present invention is that the existing detection method of dabigatran etexilate mesylate or its preparation related substances can only detect the degraded impurities of capsules, and many related substances impurities cannot be detected

Method used

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  • Method for detecting related substances or/and content thereof for dabigatran etexilate mesylate and dabigatran etexilate mesylate preparations
  • Method for detecting related substances or/and content thereof for dabigatran etexilate mesylate and dabigatran etexilate mesylate preparations
  • Method for detecting related substances or/and content thereof for dabigatran etexilate mesylate and dabigatran etexilate mesylate preparations

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Experimental program
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Effect test

Embodiment 1

[0044] Chromatographic conditions and system suitability test Use octadecylsilane bonded silica gel as a filler (Phenomenex Gemini C18, 4.6×250mm, 5μm recommended), 0.2% ammonium acetate solution (glacial acetic acid to adjust the pH to 4.3) It is mobile phase A and acetonitrile as mobile phase B. Gradient elution is carried out according to the following table; the column temperature is 35°C, the flow rate is 1.0ml / min, and the detection wavelength is 242nm, 310nm, 340nm.

[0045]

[0046] Take the impurity 6 reference substance, accurately weigh it, dissolve it with diluent 1 [acetonitrile-ethanol-water (12:3:10)] and dilute with diluent 2 [mobile phase A-mobile phase B(85:15)] to make Each 1ml contains about 0.3mg of the solution as the reference solution (1); accurately weigh impurity 02, impurity 5, impurity 7, impurity 9, impurity 1, impurity 2, impurity 4, impurity 8, impurity 10, impurity 11. For each reference substance of impurity 12, dissolve it with the above diluent ...

Embodiment 2

[0053] Chromatographic conditions and system suitability test Use octadecyl silane bonded silica gel as a filler (Phenomenex Gemini C18, 4.6×250mm, 5μm recommended), 0.3% ammonium acetate solution (glacial acetic acid to adjust the pH to 4.3) It is mobile phase A and acetonitrile as mobile phase B. Gradient elution is performed according to the following table; the column temperature is 35°C, the flow rate is 1.0ml / min, and the detection wavelength is 242nm, 310nm, 340nm.

[0054]

[0055]

[0056] Take the impurity 6 reference substance, accurately weigh it, dissolve it with diluent 1 [acetonitrile-ethanol-water (12:3:10)] and dilute with diluent 2 [mobile phase A-mobile phase B(85:15)] to make Each 1ml contains about 0.3mg of the solution as the reference solution (1); accurately weigh impurity 02, impurity 5, impurity 7, impurity 9, impurity 1, impurity 2, impurity 4, impurity 8, impurity 10, impurity 11. For each reference substance of impurity 12, dissolve it with the above ...

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Abstract

The invention relates to a method for detecting the related substances or / and content thereof for dabigatran etexilate mesylate and dabigatran etexilate mesylate preparations. According to the detection method, high performance liquid chromatography is adopted. The following method conditions are adopted: an anti-phase silica gel chromatographic column is adopted as an chromatographic column; detection wavelengths range from 210 to 400nm; mobile phases include a mobile phase A and a mobile phase B; the mobile phase A is an aqueous phase containing a buffer solution; the pH of the mobile phaseA ranges from 4.25 to 4.40; the mobile phase B mainly comprises methanol or acetonitrile; and the mobile phases are eluted with a gradient elution method. With the detection method of the invention adopted, the chromatographic peaks of the related substances of the dabigatran etexilate mesylate and the dabigatran etexilate mesylate preparations can be separated, and therefore, high chromatographicpeak resolution can be realized.

Description

Technical field [0001] The present invention relates to the field of detection methods for related substances, in particular to a detection method for related substances or / and content of dabigatran etexilate mesylate or its preparations. Background technique [0002] Dabigatran etexilate mesylate was developed by Boehringer Ingelheim, Germany. It was first approved by the US Food and Drug Administration in 2010 for the prevention of stroke and systemic embolism in patients with non-valvular atrial fibrillation. It is a direct thrombin inhibitor , A prodrug of dabigatran, a non-peptide thrombin inhibitor, the latter is released in the body after oral administration, and binds to the fibrin-specific site of thrombin to prevent fibrinogen from cleaving into fibrin, thereby preventing The final step of breaking the blood clotting waterfall network and thrombosis, the drug market, is a major progress in the field of anticoagulation therapy and the field of potentially fatal thrombosi...

Claims

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Application Information

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IPC IPC(8): G01N30/02G01N30/34G01N30/74
CPCG01N30/02G01N30/34G01N30/74
Inventor 陈翠翠葛志乐罗鸣赵同华周巍何威轩李英富苏忠海
Owner CHENGDU BRILLIANT PHARMA CO LTD
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