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Method for detecting impurities in formoterol fumarate or related preparations thereof

A technology of formoterol fumarate and impurities, applied in measuring devices, instruments, scientific instruments, etc., can solve problems such as poor reproducibility of test results, short service life of chromatographic columns, lack of diastereoisomers, etc. Achieve excellent reproducibility, low price, and make up for the effect of diastereomer impurity content

Active Publication Date: 2019-10-25
GUANGZHOU JOINCARE RESPIRATORY DRUG ENG TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] However, the above method has the following disadvantages in practical application: 1) the chromatographic column using octadecyl bonded polyvinyl alcohol as the stationary phase has poor tolerance and short service life in this method; 2) due to the octadecyl bond Synthesized polyvinyl alcohol is the chromatographic column of stationary phase poor tolerance in this method, causes after the chromatographic column is used for a long time, the reproducibility of detection result is poor; The only manufacturer of the column is Showa Denko Co., Ltd., which is expensive, and alternative products are scarce, and the use cost of enterprises is high, which restricts the development of the industry
[0008] Therefore, in the method for detecting non-enantiomers of formoterol fumarate disclosed in the prior art, there are defects such as short service life of the chromatographic column, poor reproducibility of detection results, and high application cost of the method.
In addition, there is a lack of methods in the art that can detect diastereoisomers in related formulations of formoterol fumarate

Method used

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  • Method for detecting impurities in formoterol fumarate or related preparations thereof
  • Method for detecting impurities in formoterol fumarate or related preparations thereof
  • Method for detecting impurities in formoterol fumarate or related preparations thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0074] Detection conditions:

[0075] Take carbooctadecylsilane bonded phase chromatographic column Waters XBridge C18 (250mm×4.6mm, 5μm); A solution is (0.6%, V / V) tetrabutylammonium hydroxide water-soluble (phosphoric acid to adjust pH=8.5), B solution It is acetonitrile, the volume ratio of solution A to solution B is 80:20; column temperature: 35°C; flow rate: 1.0mL / min; detection wavelength: 225nm; injection volume: 50μL.

[0076] Experimental steps:

[0077] Preparation of blank solution (diluent):

[0078] Measure 120ml of acetonitrile and 880ml of water respectively, shake well, and obtain.

[0079] Preparation of system suitability solution:

[0080] Weigh about 2 mg of formoterol fumarate impurity I identification reference substance (EDQM, European official reference substance), put it in a 20ml measuring bottle, add diluent to dissolve and dilute to the mark, shake well, and obtain.

[0081] Preparation of the test solution:

[0082] Take 1 bottle of formotero...

Embodiment 2

[0086] Detection condition: with embodiment 1.

[0087] Experimental steps:

[0088] The preparation of blank solution (diluent), system suitability solution, need testing solution: with embodiment 1.

[0089] Impurity I positioning solution:

[0090] Weigh about 14mg of formoterol fumarate impurity I reference substance (EDQM), put it in a 20ml measuring bottle, add diluent to dissolve and dilute to the mark, shake well, and obtain.

[0091] Impurity A positioning solution:

[0092] Weigh about 1mg of formoterol fumarate impurity A (source: TLC company) reference substance into a 100ml measuring bottle, add diluent to dissolve and dilute to the mark, shake well, and precisely pipette 1ml of the solution into a 10ml measuring bottle , dilute to the mark with diluent, shake well, and get it.

[0093] Determination:

[0094] Inject one needle each of the system suitability solution, the test solution, the impurity I localization solution, and the impurity A localization sol...

Embodiment 3

[0099] Detection condition: with embodiment 1.

[0100] Experimental steps:

[0101] Preparation of blank solution (diluent) and system suitability solution: same as in Example 1.

[0102] Preparation of the test solution:

[0103] Precisely weigh 7mg of formoterol fumarate raw material, put it in a 100ml volumetric flask, add diluent to dilute and dissolve and dilute to the scale, shake well, and you get it;

[0104] Determination:

[0105] Take blank solution, system suitability solution and test solution and inject one needle each. Carry out high performance liquid chromatography analysis by above-mentioned condition, record chromatogram, calculate formoterol fumarate impurity I content by peak area normalization method. Result shows, the content of the impurity I of this batch need testing product is 0.14%, and HPLC chromatogram sees attached image 3 , image 3 A is the spectrum of the blank solution, image 3 B is the system suitability solution spectrum, image ...

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Abstract

The present invention provides a method for detecting impurities in formoterol fumarate or related preparations thereof. The method comprises a step of detecting diastereoisomer impurities (impuritiesI) in the formoterol fumarate or related preparations by using a high performance liquid chromatography method, wherein an eluent used in the high performance liquid chromatography is a system consisting of a liquid A and a liquid B, the liquid A is an ion pair reagent buffer, the liquid B is acetonitrile, and the elution mode is isocratic elution. The method of the invention has the advantages of good tolerance, long service life, the good reproducibility of a detection result, and multiple types of optional columns, and the reduction of the application cost. A measurement result obtained bythe method of the invention is accurate, and the method can be simultaneously applied to the detection of the content of diastereoisomer impurities in a formoterol fumarate crude drug and related preparations.

Description

technical field [0001] The invention relates to the technical field of drug detection, in particular to a method for detecting impurities in formoterol fumarate or its related preparations. Background technique [0002] Formoterol Fumarate is a β2-adrenoceptor agonist developed by Yamanouchi Pharmaceutical Co., Ltd., Japan, for the treatment of bronchial asthma, acute bronchitis or asthmatic bronchitis and other airway obstructive pulmonary diseases , chemical name: (±)-N-[2-hydroxy-5-[(1RS)-hydroxy-2[[(1RS)-2-(4-methoxybenzyl)-1-methylethyl] Amino] ethyl] phenyl] formamide fumarate dihydrate is a pharmaceutically acceptable salt of Formoterol (Formoterol), and its structure is as shown in formula (1): [0003] [0004] At present, the Chinese guidelines for asthma prevention, the American Thoracic Society (ATS) and the European Respiratory Society (ERS) have listed formoterol fumarate as the preferred long-acting β2 receptor agonist as a bronchodilator for controlling a...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02G01N30/34
CPCG01N30/02G01N30/34
Inventor 文景兵钟凤萍金方
Owner GUANGZHOU JOINCARE RESPIRATORY DRUG ENG TECH CO LTD
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