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Method for detecting bromomethane in 7-azoniabicyclo [2.2.1] heptane derivative

A detection method and derivative technology, applied in the direction of measuring devices, instruments, scientific instruments, etc., to achieve the effect of improving safety, good specificity, and high accuracy

Active Publication Date: 2021-03-09
SHANDONG LUKANG PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

7-azonium bicyclo[2.2.1]heptane derivatives and other anticholinergics with similar structures are suitable for patients with COPD, who are characterized by life-long medication, but there is no 7-azonium bicyclo[2.2.1] Related reports on the detection method of methyl bromide in anticholinergic drugs with similar structures such as heptane derivatives

Method used

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  • Method for detecting bromomethane in 7-azoniabicyclo [2.2.1] heptane derivative
  • Method for detecting bromomethane in 7-azoniabicyclo [2.2.1] heptane derivative
  • Method for detecting bromomethane in 7-azoniabicyclo [2.2.1] heptane derivative

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0042] Example 1 Detection of methyl bromide in 7-azonium bicyclo[2.2.1]heptane derivatives

[0043] Preparation of reference substance solution: Accurately weigh an appropriate amount of methyl bromide reference substance, add ethanol-ether (the volume ratio of ethanol and ether is 2:1) to dissolve and quantitatively dilute to make a solution containing 0.045 mg of methyl bromide per 1 mL, as a reference substance solution.

[0044] Preparation of the test solution: Take an appropriate amount of 7-azonium bicyclo[2.2.1]heptane derivative, accurately weigh it, add ethanol-ether (the volume ratio of ethanol and ether is 2:1) to dissolve and quantitatively dilute to prepare each A solution containing 15 mg of 7-azonium bicyclo [2.2.1] heptane derivatives in 1 mL was used as the test solution.

[0045] Accurately measure each 1 μ L of reference substance solution and need testing solution respectively, inject gas chromatograph, record peak area, measure the content of methyl bro...

Embodiment 2

[0048] Embodiment 2 methodological verification

[0049] 1. Exclusiveness

[0050] Prepare reference substance solution and need testing solution according to the method in Example 1, and take ethanol-ether (the volume ratio of ethanol and ether is 2:1) as blank solution;

[0051] Preparation of standard-added test solution: Take an appropriate amount of 7-azonium bicyclo[2.2.1]heptane derivative, accurately weigh it, add reference substance solution to dissolve and quantitatively dilute to make about 7-azonium bicyclo [2.2.1] A solution of 15 mg of heptane derivatives is used as a standard-added test solution.

[0052] Accurately measure 1 μL each of the blank solution, the reference solution, the test solution, and the spiked test solution under the "repeatability" item, inject it into the gas chromatograph, and record the retention time, peak area and separation of methyl bromide in the chromatogram. The results are shown in Table 2.

[0053] Table 2 Methodological verif...

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Abstract

The invention relates to the technical field of pharmacy, and provides a method for detecting bromomethane in a 7-azoniabicyclo [2.2.1] heptane derivative. According to the scheme, bromomethane is used as a reference substance, gas chromatography is used for detecting the content of bromomethane in the 7-azoniabicyclo [2.2.1] heptane derivative, and the content of bromomethane in the 7-azoniabicyclo [2.2.1] heptane derivative is calculated through an external standard method. Methodological verification shows that the detection method provided by the invention is high in sensitivity and accuracy and good in specificity, can be used for effectively detecting whether the 7-azoniabicyclo [2.2.1] heptane derivative contains residual bromomethane or not and accurately measuring the content of the bromomethane, and can be used for effectively controlling the quality of a 7-azoniabicyclo [2.2.1] heptane derivative product; and the safety of a medicament is increased.

Description

technical field [0001] The invention relates to the technical field of pharmacy, in particular to a detection method for methyl bromide in 7-azonium bicyclo[2.2.1]heptane derivatives. Background technique [0002] (1R,2S)-2-((R)-2'-cyclopentyl-2'-hydroxy-2'-phenylacetoxy)-7,7-dimethyl-7-azabicyclo[2.2 .1] Heptane bromide (referred to as 7-azonium bicyclo[2.2.1]heptane derivative) is a highly effective and selective muscarinic receptor antagonist for bronchospasm with chronic obstructive pulmonary disease Long-term maintenance treatment of disease (COPD). The 7-azonium bicyclo[2.2.1]heptane derivative has a similar structure to anticholinergic drugs such as tiotropium bromide, ipratropium bromide, and glycopyrronium bromide. [0003] Methyl bromide, also known as methyl bromide, is a methyl halide compound, often used as a synthetic raw material for anticholinergic drugs, such as tiotropium bromide, ipratropium bromide, glycopyrronium bromide, etc. It is also a 7-azonium bi...

Claims

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Application Information

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IPC IPC(8): G01N30/02G01N30/06G01N30/86
CPCG01N30/02G01N30/06G01N30/8675G01N2030/047
Inventor 王喃喃刘姣崔成伟
Owner SHANDONG LUKANG PHARMA
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