A kind of detection method of impurity a in different third detropammonium bromide

A technology of ipratropium bromide and detection method is applied in the detection field of impurity A in ipratropium bromide, and achieves the effects of short detection time, realization of baseline separation and good specificity

Active Publication Date: 2021-07-27
JOINCARE HAIBIN PHARM CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] Therefore, it is urgent to develop a kind of ion chromatography technology that can effectively solve the impurity A content in the different third detropammonium bromide solution due to the inaccuracy caused by indirect calculation

Method used

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  • A kind of detection method of impurity a in different third detropammonium bromide
  • A kind of detection method of impurity a in different third detropammonium bromide
  • A kind of detection method of impurity a in different third detropammonium bromide

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0053] Example 1: Determination of Impurity A in Ipratropium Bromide by Ion Chromatography

[0054] Instrument and chromatographic conditions:

[0055] Thermo Fisher DIONEX ICS-2100 ion chromatograph;

[0056] Detector: conductivity detector;

[0057] Suppressor: Cationic Suppressor CSRS 300, 4mm;

[0058] Chromatographic column: the analytical column is IonPac CS17 4×250mm, 3.5μm; the pre-column is IonPac CG17 4×50mm;

[0059] Column temperature 35°C;

[0060] Carry out isocratic elution with 5mmol / L methanesulfonic acid aqueous solution-acetonitrile (60:40), flow rate 1.0ml / min; injection volume 500μl.

[0061] Specific detection steps:

[0062] Step 1. Preparation of the test solution: Accurately weigh 50 mg of ipratropium bromide raw material and place it in a 10ml volumetric flask, dilute to the mark with ultrapure water solvent, shake well, and you get it.

[0063] Step 2. Preparation of reference substance solution: Accurately weigh an appropriate amount of ipra...

Embodiment 2

[0067] Example 2: The specificity test of detection method of the present invention

[0068] The specificity test was carried out under the same chromatographic conditions as in Example 1.

[0069] Specific test steps:

[0070] Step 1. Preparation of blank solution, ie ultrapure water.

[0071] Step 2. The preparation of the system suitability solution is consistent with the system suitability solution in Example 1.

[0072] Step 3. The preparation of the reference substance solution is consistent with the reference substance solution in Example 1.

[0073] Step 4. Sample spiked solution: Precisely weigh 50 mg of the sample and place it in a 10ml volumetric flask, dissolve it with the reference solution to make up the volume, and shake well to get it.

[0074] Step 5. Preparation of positioning solution: take an appropriate amount of sodium chloride and dissolve and dilute it with ultrapure water to obtain a sodium ion positioning solution; take an appropriate amount of p...

Embodiment 3

[0078] Example 3: The linear range test of detection method of the present invention

[0079] The same method as in Example 1 was used to carry out the linear range test.

[0080] The results showed that the impurity A of ipratropium bromide was in the concentration range of L-200% (0.5-10μg / ml), and the concentration was taken as the abscissa, and the peak area was taken as the ordinate to carry out linear regression, and the linear correlation coefficient r was 0.9993. It shows that the method of the present invention has a good linear relationship in the concentration range of L-200% (0.5-10 μg / ml), and is suitable for the quantitative detection of trace ipratropium bromide impurity A.

[0081] The linear range test method in this embodiment belongs to the prior art.

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Abstract

The invention provides a method for detecting impurity A in ipratropium bromide, said method comprising the following steps: (1) preparing a reference substance solution: accurately weighing an appropriate amount of ipratropium bromide impurity A reference substance, and using ultra-pure Dissolve and dilute with water to make a reference substance solution containing about 5 μg of ipratropium bromide impurity A in every 1ml; Dissolve in pure water and dilute to the mark, shake well, and you get it; (3) Detection: Precisely draw 500 μl of the reference solution prepared in step (1) and the test solution prepared in step (2) and inject it into a chromatographic column equipped with a cation measured in an ion chromatograph.

Description

technical field [0001] The invention relates to the technical field of drug analysis, in particular to a method for detecting impurity A in ipratropium bromide. Background technique [0002] Ipratropium bromide is a small molecular compound of quaternary ammonium salts containing UV-absorbing groups, which can be used not only to relieve bronchospasm and wheezing symptoms caused by chronic obstructive pulmonary disease (COPD), but also to prevent and treat asthma. In patients who have muscle tremors and tachycardia due to taking beta-agonists and thus cannot tolerate such drugs. The mother nucleus of ipratropium bromide is a quaternary ammonium salt structure containing ultraviolet absorbing groups, and many of its related impurities are also quaternary ammonium salt structures containing ultraviolet absorbing groups. However, impurity A is the only non-ultraviolet-absorbing quaternary ammonium compound among the many impurities of ipratropium bromide, so it cannot be detec...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/02G01N30/06
CPCG01N30/02G01N30/06
Inventor 陈世坤刘海钧毛小荣罗时远
Owner JOINCARE HAIBIN PHARM CO LTD
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