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Method for detecting related substance imidazole in starting material F of dabigatran etexilate mesylate

A technology for dabigatran etexilate mesylate and substance imidazole, which is applied in the field of detection of imidazole related substances in dabigatran etexilate mesylate starting material F, can solve the problem that no imidazole detection method is found and imidazole cannot be detected. To achieve the effect of accurate and reliable measurement results, rapid detection, and safety assurance

Active Publication Date: 2016-10-19
CHENGDU BAIYU PHARMA CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] The inspection method of the above-mentioned related substances refers to the internal control standard of the supplier of the starting material, and can determine ethyl 3-(pyridin-2-ylamino)propionate, 4-(methylamino)-3-nitrobenzoic acid among the above-mentioned known impurities , 3-[(3-amino-4-methylaminobenzoyl)pyridin-2-ylamino]propanoic acid, 3-[(3-nitro-4-methylaminobenzoyl)pyridine-2- Amino] ethyl propionate, but imidazole cannot be detected under the determination conditions of this related substance
After the inventor's literature search, no relevant reports were found to record the imidazole detection method

Method used

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  • Method for detecting related substance imidazole in starting material F of dabigatran etexilate mesylate
  • Method for detecting related substance imidazole in starting material F of dabigatran etexilate mesylate
  • Method for detecting related substance imidazole in starting material F of dabigatran etexilate mesylate

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Effect test

preparation example Construction

[0033] (1) Preparation of the test solution: get an appropriate amount of starting material F, accurately weighed, add mobile phase to dissolve and dilute to make a solution containing 0.5-2 mg (preferably 1 mg / ml) of starting material F in every 1 ml, As the test solution;

[0034] (2) Preparation of reference substance solution:

[0035] Take an appropriate amount of imidazole, accurately weighed, add mobile phase to dissolve and dilute to make a solution containing 0.5-5 μg (preferably 1 μg / ml) per 1 ml, as a reference solution.

Embodiment 1

[0037] The detection method of imidazole adopts liquid chromatography detection, and HPLC detection condition is as follows:

[0038] Chromatographic column: Shimadzu C18 (250mm×4.6mm 5μm)

[0039] Mobile Phase A: Water

[0040] Mobile Phase B: Acetonitrile

[0041] Isocratic elution: mobile phase A: mobile phase B (90:10); run for 50min, flow rate 1.0mL / min, column temperature: 35°C, injection volume: 10μL, detection wavelength: 210nm.

[0042] Result: The main peak is not retained, the peak shape is poor, the blank interferes with the detection, and then optimized.

Embodiment 2

[0044] The detection method of imidazole adopts liquid chromatography detection, and HPLC detection condition is as follows:

[0045] Chromatographic column: Shimadzu C18 (250mm×4.6mm 5μm)

[0046] Mobile phase A: 0.02mol / L potassium dihydrogen phosphate (phosphoric acid adjusted to PH4.0)

[0047] Mobile Phase B: Acetonitrile

[0048] Isocratic elution: mobile phase A: mobile phase B (90:10); run for 50min, flow rate 1.0mL / min, column temperature: 35°C, injection volume: 10μL, detection wavelength: 210nm.

[0049] Result: The main peak is not retained, the peak shape is poor, the blank interferes with the detection, and then optimized.

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Abstract

The invention belongs to field of pharmaceutical analysis, and more specifically relates to a method for detecting a related substance imidazole in a starting material F of dabigatran etexilate mesylate. The method which can be operated simply, rapidly and accurately is used for detecting the related substance imidazole in the starting material F; concretely, liquid chromatogram is employed for detection, and key HPLC detection conditions are controlled: the proportion between a mobile phase acetonitrile and water is 10-30:90-100, an amide-bonded silica gel chromatographic column is used, and the detection wavelength is 200-230nm. Key detection parameters are controlled in order to realize the purposes of simple, rapid and accurate detection, and the method can be simply operated; the detection result is accurate and reliable; the specificity is good; the retention time of the starting material F is 3-4 minutes, the retention time of imidazole is 6-7 minutes, the detection time is short, and a brand new selection is provided for detecting related substances in the product, controlling product quality, and guarantying safety of medicines.

Description

technical field [0001] The invention belongs to the field of drug analysis, in particular to a method for detecting imidazole, a related substance in dabigatran etexilate mesylate starting material F. Background technique [0002] The name of the starting material F of dabigatran etexilate mesylate is 3-[(3-amino-4-methylaminobenzoyl) pyridin-2-ylamino] ethyl propionate, and the structure is as follows: [0003] [0004] Known impurity situation analysis in the dabigatran etexilate mesylate starting material F is as follows: [0005] Analysis of impurities [0006] [0007] The inspection method of the above-mentioned related substances refers to the internal control standard of the supplier of the starting material, and can determine ethyl 3-(pyridin-2-ylamino)propionate, 4-(methylamino)-3-nitrobenzoic acid among the above-mentioned known impurities , 3-[(3-amino-4-methylaminobenzoyl)pyridin-2-ylamino]propanoic acid, 3-[(3-nitro-4-methylaminobenzoyl)pyridine-2- Ami...

Claims

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Application Information

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IPC IPC(8): G01N30/02
Inventor 黎小平胡小明蒋忠君孙毅
Owner CHENGDU BAIYU PHARMA CO LTD
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