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Method for detecting related substances of 2-bromomethyl-1, 3-dioxopentane

A technology of dioxolane and detection method, applied in the field of chemical analysis, can solve problems such as lack of effective detection, and achieve the effects of quality control, simple operation and high specificity

Active Publication Date: 2022-07-08
SHIJIAZHUANG NO 4 PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] Aiming at the technical problem of lack of effective detection of related substances in 2-bromomethyl-1,3-dioxolane in the prior art, the present invention provides a Determination method for related substances of 2-bromomethyl-1,3-dioxolane

Method used

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  • Method for detecting related substances of 2-bromomethyl-1, 3-dioxopentane
  • Method for detecting related substances of 2-bromomethyl-1, 3-dioxopentane
  • Method for detecting related substances of 2-bromomethyl-1, 3-dioxopentane

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0040] 1.1 Preparation of solution:

[0041] Blank solvent: N,N-dimethylformamide.

[0042] Preparation of mixed reference solution: take vinyl acetate, 2-bromo-1,1-dimethoxyethane, 2-methyl-1,3-dioxolane and 2-bromoethyl acetate as controls Appropriate amount of the product, accurately weighed, and quantitatively diluted with N,N-dimethylformamide to prepare approximately vinyl acetate, 2-bromo-1,1-dimethoxyethane, 2-methyl- 1,3-dioxolane and 2-bromoethyl acetate each 500μg solution, as mixed reference solution.

[0043] Preparation of the test solution: take 1.0 g of 2-bromomethyl-1,3-dioxopentane sample, accurately weigh it, place it in a 10 mL volumetric flask, and prepare the concentration with N,N-dimethylformamide For the 100mg / mL test solution.

[0044] Preparation of the solution for adding the standard test solution: take 1.0 g of 2-bromomethyl-1,3-dioxopentane sample, accurately weigh it, place it in a 10 mL volumetric flask, and accurately add 5000 μg of vinyl a...

Embodiment 2

[0055] Methodological validation:

[0056] 2.1 Exclusivity

[0057] Take the blank solvent, the above-mentioned mixed reference solution and the standard solution for testing according to the above-mentioned gas chromatographic conditions, and record the chromatogram. The results are as follows: Figure 1-Figure 3 shown, where, figure 1 is the chromatogram of the blank solvent, figure 2 is the chromatogram of the mixed reference solution, image 3 For the chromatogram of the spiked test solution. The test results of the separation degree of each component are shown in Table 1-Table 2.

[0058] Table 1 Test results of the separation degree of each component in the mixed control solution

[0059] Element Retention time (min) degree of separation vinyl acetate 3.571 -- 2-Methyl-1,3-dioxolane 4.785 15.328 2-Bromo-1,1-dimethoxyethane 9.771 59.042 2-Bromoethyl acetate 10.320 7.396

[0060] Table 2 The separation degree of each com...

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Abstract

The invention relates to the technical field of chemical analysis, and particularly discloses a method for detecting related substances of 2-bromomethyl-1, 3-dioxopentane. DB-624UI (30m * 0.32 mm * 1.8 [mu] m) is adopted as a detection chromatographic column, the column temperature is set to be 38-42 DEG C and maintained for 2-5 min, then the temperature is increased to 110-130 DEG C at the rate of 9-11 DEG C / min, then the temperature is increased to 245-255 DEG C at the rate of 49-51 DEG C / min and maintained for 2-5 min, the temperature of a sample inlet is 255-265 DEG C, the temperature of a detector is 245-255 DEG C, and the split ratio is 3-10: 1, so that the detection of 2-bromomethyl-1, 3, 5-trimethyl-1, 3, 5-trimethyl-1, 3, 5-trimethyl-1, 3, 5-trimethyl-1, 3, 5-trimethyl-1, 3, 5- According to the present invention, the simultaneous quantitative detection of a variety of known impurities and unknown impurities in 2-bromomethyl-1, 3-dioxopentane can be achieved, such that the real reflection of the quality of 2-bromomethyl-1, 3-dioxopentane can be easily achieved so as to easily achieve the quality control of the doxofylline product.

Description

technical field [0001] The invention relates to the technical field of chemical analysis, in particular to a method for detecting 2-bromomethyl-1,3-dioxolane related substances. Background technique [0002] 2-Bromomethyl-1,3-dioxopentane is an important starting material in the synthesis of doxofylline, and it contains a warning structure of a genotoxic carcinogenic impurity, classified by ICH M7 as a genotoxic impurity 3, which may become a genotoxic impurity. Causes of cancer. [0003] At present, the main process route for synthesizing 2-bromomethyl-1,3-dioxolane is as follows, using vinyl acetate, methanol and bromine water as raw materials to prepare 2-bromo-1,1-dimethoxyethane, Then 2-bromo-1,1-dimethoxyethane and ethylene glycol react under the catalysis of p-toluenesulfonic acid to generate 2-bromomethyl-1,3-dioxolane. During the reaction, various impurities such as vinyl acetate, 2-bromo-1,1-dimethoxyethane, 2-methyl-1,3-dioxolane and 2-bromo Ethyl acetate. The...

Claims

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Application Information

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IPC IPC(8): G01N30/02G01N30/06G01N30/86
CPCG01N30/02G01N30/06G01N30/8679G01N2030/065
Inventor 毕贺宗莹莹杨俊免孙朝利马明卓陈碧楚赵杨王亚静韩倩茹骆会茹相雅婷祝春英
Owner SHIJIAZHUANG NO 4 PHARMA
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