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Method for separating and determining 2,4-dichloroacetophenone and 2,6-dichloroacetophenone isomers by high-performance liquid chromatography

A kind of technology of high performance liquid chromatography and dichloroacetophenone, applied in the field of analytical chemistry, can solve the problems such as separation and measurement not seen in literature reports and the like

Inactive Publication Date: 2018-08-24
常州市盛辉药业有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

At present, there is no literature report on the separation and determination of 2,4-dichloroacetophenone and 2,6-dichloroacetophenone isomers

Method used

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  • Method for separating and determining 2,4-dichloroacetophenone and 2,6-dichloroacetophenone isomers by high-performance liquid chromatography
  • Method for separating and determining 2,4-dichloroacetophenone and 2,6-dichloroacetophenone isomers by high-performance liquid chromatography
  • Method for separating and determining 2,4-dichloroacetophenone and 2,6-dichloroacetophenone isomers by high-performance liquid chromatography

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Embodiment 1

[0024] 1. Instrument

[0025] High performance liquid chromatography: Shimadzu, LC-20AT, SPD-20A UV-Vis detector.

[0026] Chromatographic column: Kromasil C18 (4.6*250nm*5μm).

[0027] 2. Chromatographic conditions

[0028] Mobile phase composition volume ratio: methanol: water = 70:30;

[0029] Flow rate: 1.0mL / min;

[0030] Detection wavelength: 220nm;

[0031] Column temperature: 25°C;

[0032] Injection volume: 20 μL.

[0033] 3. Experimental steps

[0034] Weigh 5g of 2,4-dichloroacetophenone and 5g of 2,6-dichloroacetophenone into a 100mL volumetric flask, dissolve and dilute to the mark with ethanol solution, and shake well. Obtain a sample solution.

[0035] Take 20 μL of the above solution, analyze according to the above chromatographic conditions, and record the chromatogram, the results are as follows: figure 1 shown.

[0036] figure 1 The chromatographic peak with a retention value of 7.934min is 2,4-dichloroacetophenone, and the chromatographic peak wi...

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Abstract

The invention discloses a method for separating and determining 2,4-dichloroacetophenone and 2,6-dichloroacetophenone isomers by high-performance liquid chromatography. According to the method disclosed by the invention, a C18 reversed phase chromatographic column is adopted, and a mixed solution of methanol and water is used as a mobile phase; the volume ratio of the methanol to the water in themobile phase is (90 to 70) to (10 to 30); the flow speed of the mobile phase is 0.8 to 1.2mL / min, the detection wavelength is 220nm, the temperature of the chromatographic column is 10 to 50 DEG C andthe sample feeding amount is 0.5 to 100muL; separation of 2,4-dichloroacetophenone and 2,6-dichloroacetophenone is realized, and chromatographic conditions are provided for quantitative detection ofthe 2,4-dichloroacetophenone and the 2,6-dichloroacetophenone.

Description

technical field [0001] The invention belongs to the technical field of analytical chemistry, and in particular relates to a method for separating and measuring 2,4-dichloroacetophenone and 2,6-dichloroacetophenone isomers by high performance liquid chromatography. Background technique [0002] 2,4-Dichloroacetophenone is a light yellow solid, an important fine chemical intermediate, widely used in medicine, pesticide and other fields. It is the first clinically available oral broad-spectrum antifungal drug ketoconazole [cis-[2-(2,4-dichloro)-2-(1H-imidazolyl-1-methanol) Base)-1,3-dioxolane-4-]methyl p-toluenesulfonate (active ester) intermediate is an important raw material. [0003] Because inevitably can produce a certain amount of 2,6-dichloroacetophenone (isomers) in the synthetic process of 2,4-dichloroacetophenone, the 2,6-dichloroacetophenone The purity of 2,4-dichloroacetophenone is affected, thereby affecting the synthetic effect of ketoconazole. [0004] The sep...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/89
CPCG01N30/89
Inventor 陈舟
Owner 常州市盛辉药业有限公司
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