Method for detecting content of ipratropium bromide intermediate I and related substances

A technology of ipratropium bromide and related substances, which is applied in the detection field of content and related substances, and achieves the effects of good repeatability, good specificity and sensitivity, and simple and convenient operation process

Pending Publication Date: 2020-10-09
TIANJIN PHARMA GROUP CORP
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0006] After literature research, no literature or pharmacopoeia was found to report and record the method for the determination of the external isomer of the reduced product of ipratropium bromide intermediate

Method used

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  • Method for detecting content of ipratropium bromide intermediate I and related substances
  • Method for detecting content of ipratropium bromide intermediate I and related substances
  • Method for detecting content of ipratropium bromide intermediate I and related substances

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Experimental program
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Effect test

Embodiment 6

[0041] The system suitability solution of embodiment 6: take 9.0mg of reducing substance, 1.0mg of exoisomer, accurately weighed, put in 10ml measuring bottle, add mobile phase solution and dilute to volume, shake well, as system suitability solution.

Embodiment 7

[0042] Example 7 Sample injection for the test product.

[0043] Comparative example 1-2 sample injection is system suitability solution

Embodiment 1

[0044] Embodiment 1 system suitability test

[0045] Chromatographic conditions:

[0046] Chromatographic column: Propanylsilane bonded silica gel column (3.0×150mm, 3.5μm)

[0047] Mobile phase A: Add 5.0g potassium dihydrogen phosphate, 1.36g tetrapropylammonium chloride, 8ml triethylamine to 1L water, adjust the pH to 5.0 with phosphoric acid;

[0048] Mobile Phase B: Acetonitrile

[0049] Mobile phase A: mobile phase B = 95:5

[0050] Detection wavelength: 220nm Column temperature: 50°C

[0051] Flow rate: 1.0ml / min Injection volume: 10μl

[0052] Test results: see figure 1

[0053] name keep time Separation reduced exoisomer 6.328 reduction 6.995 1.7

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Abstract

The invention provides a method for detecting the content of an ipratropium bromide intermediate I and related substances. High performance liquid chromatography is adopted, propyl silane bonded silica gel serves as a chromatographic column, a mobile phase is composed of a phase A and a phase B, a phosphate buffer solution containing cation pairs serves as a mobile phase A, acetonitrile serves asa mobile phase B, the ratio of the mobile phase A to the mobile phase B is 90-98: 2-10, an ultraviolet detector is adopted, and the detection wavelength ranges from 210 nm to 230 nm. The method disclosed by the invention has the beneficial effects that the method can be used for rapidly and accurately detecting the exterior isomer impurities in the reduction product and has good specificity and sensitivity, the mobile phase is cheap and easy to obtain, the operation process is simple and convenient, and the accuracy and repeatability are good.

Description

technical field [0001] The invention belongs to the field of medicines, in particular to a method for detecting the content of ipratropium bromide intermediate I and related substances. Background technique [0002] Ipratropium bromide is a potent anticholinergic drug with high selectivity to bronchial smooth muscle M receptors. It has a strong effect on relaxing bronchial smooth muscle and a weak effect on respiratory glands and cardiovascular system. It is used to relieve bronchospasm and wheezing symptoms caused by chronic obstructive pulmonary disease (COPD); to prevent and treat asthma, especially for patients who cannot tolerate such drugs due to muscle tremors and tachycardia caused by β-receptor agonists. [0003] [0004] With the improvement of the level of drug research and development and the increasing attention to the adverse reactions of related preparations, the attention of pharmaceutical regulatory agencies to related substances in preparation products i...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02G01N30/34G01N30/74G01N30/30G01N30/32G01N30/86
CPCG01N30/02G01N30/34G01N30/74G01N30/30G01N30/32G01N30/8637G01N2030/324
Inventor 李晓东王宏侠郭志强
Owner TIANJIN PHARMA GROUP CORP
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