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Method for detecting acryloyl chloride and related substances thereof

A detection method and technology for related substances, which are applied in measurement devices, instruments, scientific instruments, etc., can solve the problems of inability to perform accurate quantification, inability to judge gas chromatography, and difficulty in directly detecting the content.

Pending Publication Date: 2021-11-19
CHENGDU BRILLIANT PHARMA CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] Acryloyl chloride is active in chemical properties and will react with water, alcohol, and amine solvents, so it is difficult to directly detect its content
At present, the detection method for acryloyl chloride content is mainly gas chromatography. Acryloyl chloride is first derivatized with alcohol or amine (mainly aniline) compounds, and then detected by gas chromatography, but the detection by gas chromatography will miss a certain Some unknown impurities, and at the same time, it is impossible to judge that some unknown peaks in the gas chromatography are solvent peaks or impurity peaks, and accurate quantification cannot be performed
At present, there is no report on the detection method of related substances of acryloyl chloride

Method used

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  • Method for detecting acryloyl chloride and related substances thereof
  • Method for detecting acryloyl chloride and related substances thereof
  • Method for detecting acryloyl chloride and related substances thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0038] Take an appropriate amount of this product, weigh it accurately, put it in a 50ml measuring bottle, dilute to the mark with acetonitrile, and make a solution containing about 0.5mg of acryloyl chloride per 1ml, as the stock solution of the test sample.

[0039] Precisely measure 0.2ml of N-ethylaniline, put it in a 50ml measuring bottle, dilute to the mark with acetonitrile, and use it as N-ethylaniline stock solution.

[0040] Precisely measure 1ml of the stock solution of the test sample and 1ml of the N-ethylaniline stock solution, put it in a 10ml measuring bottle, shake well, leave it at room temperature for 20min, dilute with water to the mark, and use it as the test solution.

[0041] Take an appropriate amount of acryloyl chloride reference substance, weigh it accurately, dilute to the mark with acetonitrile to make a solution containing about 1 mg of acryloyl chloride per 1 ml, and use it as the stock solution of acryloyl chloride reference substance.

[0042] ...

Embodiment 2

[0068] Mobile phase A: phosphoric acid water (pH3.00), mobile phase B: acetonitrile: methanol (1:1), sample volume

[0069] 25 μl, the mobile phase elution gradient is as follows, and other conditions are the same as in Example 1:

[0070]

[0071] For chromatogram see figure 2 .

[0072] No baseline separation was achieved between the SM3-Z3 derived product and the subsequent unknown impurity.

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Abstract

The invention provides a method for detecting acryloyl chloride and related substances thereof, which takes an aniline substance as a derivatization reagent and uses high performance liquid chromatography for detection. At present, reports for detecting acryloyl chloride and / or related substances thereof through liquid chromatography do not exist, N-ethylaniline is adopted as a derivatization reagent, operation is easy and convenient, derivatization time is short, sensitivity is high, and side reactions are few; an ultraviolet detector is adopted, and in liquid chromatography detection, the application range is wide, known impurities and unknown impurities existing in a sample can be detected, and the repeatability and durability are very good.

Description

technical field [0001] The invention belongs to the field of drug analysis and relates to an HPLC detection method for acryloyl chloride and its related substances. Background technique [0002] Acryloyl chloride, colorless and flammable liquid, corrosive and irritating, volatile. Due to its active chemical properties, various types of chemical reactions can occur, and then various types of organic compounds can be derived, such as acrylate and acrylamide compounds, which are important raw materials for pharmaceutical, chemical and other industries. [0003] Acryloyl chloride is chemically active and will react with water, alcohol, and amine solvents, so it is difficult to directly detect its content. At present, the detection method for the content of acryloyl chloride is mainly gas chromatography. First, the acryloyl chloride is derivatized with alcohol or amine (mainly aniline) compounds, and then detected by gas chromatography, but the detection by gas chromatography wi...

Claims

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Application Information

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IPC IPC(8): G01N30/02G01N30/06G01N30/86
CPCG01N30/02G01N30/06G01N30/8679G01N2030/067Y02P20/55
Inventor 唐欢刘敏胡崇琳段雨晴张永红罗鸣黄浩喜苏忠海
Owner CHENGDU BRILLIANT PHARMA CO LTD
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