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Method for detecting ethyl p-toluenesulfonate and isopropyl p-toluenesulfonate in dabigatran etexilate bulk drug or preparation

A technology of isopropyl toluenesulfonate and ethyl toluenesulfonate, which is applied in the field of pharmaceutical analysis, can solve the problems of unreported content determination methods, and achieve the effects of high sensitivity, simple operation and accurate detection results

Pending Publication Date: 2022-03-01
SHIJIAZHUANG PHARMA GRP NBP PHARMA CO LTD +1
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] Yet, the method for content determination of ethyl p-toluenesulfonate and isopropyl p-toluenesulfonate in the dabigatran etexilate crude drug or preparations has not been reported at home and abroad at present

Method used

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  • Method for detecting ethyl p-toluenesulfonate and isopropyl p-toluenesulfonate in dabigatran etexilate bulk drug or preparation
  • Method for detecting ethyl p-toluenesulfonate and isopropyl p-toluenesulfonate in dabigatran etexilate bulk drug or preparation
  • Method for detecting ethyl p-toluenesulfonate and isopropyl p-toluenesulfonate in dabigatran etexilate bulk drug or preparation

Examples

Experimental program
Comparison scheme
Effect test

preparation example Construction

[0068] Preparation of blank excipient solution: Take the addition of accessories in the group in groups, hydroxypropylene, hydroxypropylcellulose, talc, and tartaric acid, mixed, plus the amount ratio of the proportion of the plug-in. 50% aqueous aqueous aqueous solution dissolved, shaken, filtered through 0.22 μm filtration membrane, and filtered into a blank excipient solution.

[0069] For ethyl p-toluenesulfonate, the formation of isopropyl toluenesulfonic acid rats: precision weighing toluenesulfonate, is about 10 mg of isopropyl toluenesulfonate, 25 ml of 10 ml of acetonitrile In the volumetric flask, add acetonitrile to the scale, shake well; 1 ml of 1ml of 1ML is taken at 100 mL of volumetric flask, add 50% aqueous aqueous solution of acetonitrile to the scale, shake well; re-eliminate 25 μl of 25mL volumetric flask, plus 50% The aqueous aqueous acetonitrile solution was diluted to the scale, shake, and obtained a solution of ethyl toluenesulfonate, the isopropyl ester con...

Embodiment 1

[0073] Example 1: Systematic Applicability

[0074] (1) Test method:

[0075] Toluene sulfonate was taken, the toluene sulfonate was used continuously injected 6-pin, recording ethyl toluenesulfonate, and isopropyl toluenesulfonic acid.

[0076] (2) Test results:

[0077] As shown in Table 1. Ethyl toluenesulfonate, the solution of toluenesulfonate is propyride, and the 6-pin RSD is 7.4%, 4.0% (standard regulations: 6-pin peak area RSD ≤ 10.0%), respectively. It indicates that the native spectrum system is good in sampling, and the systematic applicability meets the requirements.

[0078] Table 1: Example 1 System Applicability Test Results

[0079]

[0080]

Embodiment 2

[0081] Example 2: Exclusive

[0082] (1) Test method:

[0083] Samples of blank solution (50% acetonitrile aqueous solution), (Dabikitrile capsule) blank excipient solution, toluenesulfonate, isopropyl toluene sulfonic acid, Damika sulfonate .

[0084] Among them, the detection method of Dabiki group ester control solution is high performance liquid chromatography, column, flow rate, column temperature, injection volume, mobile phase A, mobile phase B, and gradient elution method as before; detection wavelength 226 nm.

[0085] (2) Test results:

[0086] As shown in Table 2, a blank solution, a blank excipient solution, a ratio of ester pair of toluenesulfonate, and there is no interference with isopropyl toluenesulfonic acid. See Figure 1-7 .

[0087] Table 2: Example 2 Experimental test results

[0088]

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Abstract

The invention aims to provide a method for detecting genotoxic impurities of ethyl p-toluenesulfonate and isopropyl p-toluenesulfonate in a dabigatran etexilate bulk drug or preparation, which adopts an ultra-high performance liquid chromatography (UPLC) and mass spectrometry combined method and comprises the following steps: (1) preparing a test solution and a reference solution; (2) taking the test solution and the reference solution, respectively injecting samples, detecting by using an ultra-high performance liquid chromatography-mass spectrometer, recording a chromatogram, and calculating the contents of ethyl p-toluenesulfonate and isopropyl p-toluenesulfonate according to an external standard method; the method is simple to operate, accurate in detection result, high in sensitivity and good in stability, and can be used for quality control of dabigatran etexilate bulk drugs or preparations.

Description

Technical field [0001] The present invention belongs to the technical field of drug analysis, and more particularly to the detection method of gene toxic impurity on toluenesulfonate in the propylene toxic impurity in the reachaarability, lycerol, isopropyl toluenesulfonic acid. Background technique [0002] Methanesulfonates - group of β-alanine, N - [[[2- [[[[[[[[[[[[[[[[[[[[[[[[[(hexoxy) carbonyl] amino] iminomethyl] phenyl] amino] Methyl] -1-methyl-1H-benzimidazole-5-yl] carbonyl] -N-2-pyrimidine - ethyl ester, methanesulfonate, its chemical structure is shown in Formula I. Grayghan developed oral direct thrombin inhibitors, mainly for: (1) prevention of stroke of patients with non-valve sexual atrial fibrillation; (2) deep venous thrombosis of patients with anti-intensive drug treatment with 5-10 days ( DVT) and pulmonary embolism (PE) prevention; (3) patients have been treated to reduce the risk of DVT and PE recurrence; (4) Prevention of DVT and PE after hip joint replacem...

Claims

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Application Information

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IPC IPC(8): G01N30/02G01N30/72G01N30/06G01N30/04G01N30/34G01N30/14G01N30/86G01N30/88
CPCG01N30/02G01N30/72G01N30/06G01N30/04G01N30/34G01N30/14G01N30/8634G01N30/88G01N2030/047G01N2030/146G01N2030/884G01N2030/8872
Inventor 王晶杜萌李晓曼白艳玲魏俊卿王津
Owner SHIJIAZHUANG PHARMA GRP NBP PHARMA CO LTD
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