A kind of detection method of p-hydroxyacetophenone related substances

A technology of p-hydroxyacetophenone and hydroxyacetophenone, which is applied in the field of drug analysis and detection, can solve problems such as unrecorded hydroxyacetophenone detection methods, and achieve the effects of improving drug safety, high sensitivity, and good reproducibility

Active Publication Date: 2022-07-12
河北广祥制药有限公司
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, at present, the pharmacopoeias of various countries have not included the detection methods of related substances of p-hydroxyacetophenone

Method used

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  • A kind of detection method of p-hydroxyacetophenone related substances
  • A kind of detection method of p-hydroxyacetophenone related substances
  • A kind of detection method of p-hydroxyacetophenone related substances

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Embodiment 1

[0035] The embodiment of the present invention provides a kind of detection method of p-hydroxyacetophenone related substances

[0036] 1.1 Materials and methods

[0037] Instruments: gas chromatograph, hydrogen flame ionization detector, measuring flask, electronic balance.

[0038] Blank solvent: 99% methanol and 1% water.

[0039] 1.2 Preparation of the solution

[0040] Reference solution: take appropriate amounts of phenol, phenol acetate, 2'-hydroxyacetophenone and 3'-hydroxyacetophenone, accurately weigh them, and prepare each 1mL reference solution with 99% methanol and 1% water. Contains 50 µg of phenol, 50 µg of phenol acetate, 50 µg of 2'-hydroxyacetophenone, and 50 µg of 3'-hydroxyacetophenone.

[0041] Test solution: Take an appropriate amount of p-hydroxyacetophenone to be tested, accurately weigh it, and use 99% methanol and 1% water to prepare 10 mg of p-hydroxyacetophenone test solution per 1 mL of test solution.

[0042] 1.3 Detection methods of p-hydroxy...

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Abstract

The invention relates to the technical field of drug analysis and detection, and specifically discloses a detection method for p-hydroxyacetophenone related substances. The invention adopts gas chromatography to measure related substances, and the chromatographic conditions are as follows: chromatographic column: a capillary column with phenyl-dimethylpolysiloxane as a fixed liquid; carrier gas flow rate: 0.5-1.5ml / min; : 8~12:1; Heating program: Initial temperature: 45~55°C, increase to 215~225°C at a rate of 8~12°C per minute, and maintain for 5~10 minutes; Inlet temperature: 240~260°C; The detector is a hydrogen flame ionization detector, and the temperature of the detector is 240-260 °C. The detection method provided by the invention can realize the effective separation of p-hydroxyacetophenone, 2'-hydroxyacetophenone, 3'-hydroxyacetophenone, phenol and phenol acetate, and accurately detect the related substances in p-hydroxyacetophenone content. In addition, the method of the invention is sensitive, accurate and reproducible, provides a reliable guarantee for improving and better controlling the quality of p-hydroxyacetophenone, and also has great significance for improving drug safety.

Description

technical field [0001] The invention relates to the technical field of drug analysis and detection, in particular to a detection method for p-hydroxyacetophenone related substances. Background technique [0002] Salbutamol sulfate is called 1-(4-hydroxy-3-hydroxymethylphenyl)-2-(tert-butylamino) ethanol sulfate, and its main function is to selectively stimulate the β2-receptors on bronchial smooth muscle to relax bronchial smooth muscle. , so as to relieve bronchial smooth muscle spasm, and has a good therapeutic effect on respiratory diseases such as bronchospasm in patients with asthmatic bronchitis, bronchial asthma and emphysema. [0003] p-Hydroxyacetophenone is an important starting material in the synthesis of salbutamol sulfate. During the synthesis of p-hydroxyacetophenone, related substances of p-hydroxyacetophenone, including isomers of p-hydroxyacetophenone, inevitably appear. 2'-Hydroxyacetophenone and 3'-hydroxyacetophenone also contain impurities such as phen...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/88
CPCG01N30/88G01N2030/884
Inventor 孙立杰韩倩茹马明卓王亚静毕贺骆会茹尹玉欣荣孜杭刘鹏赵景叶张冠华
Owner 河北广祥制药有限公司
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