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Method for separating and determining 2,4-dichloroacetophenone and o-methylacetophenone by high-performance liquid chromatography

A high-performance liquid chromatography and o-methyl acetophenone technology, applied in the field of analytical chemistry, can solve the problems of separation and determination that have not been reported in the literature

Inactive Publication Date: 2018-08-24
常州市盛辉药业有限公司
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  • 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 o-methylacetophenone

Method used

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

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Embodiment 1

[0024] This embodiment is a method for the separation and determination of 2,4-dichloroacetophenone and o-methylacetophenone by high performance liquid chromatography.

[0025] 1. Instrument

[0026] High performance liquid chromatography: Shimadzu, LC-20AT, SPD-20A UV-Vis detector.

[0027] Column: Kromasil C 18 (4.6*250nm*5μm).

[0028] 2. Chromatographic conditions

[0029] Mobile phase volume ratio: methanol: water = 70:30

[0030] Flow rate: 1.0 mL / min.

[0031] Detection wavelength: 220nm

[0032] Column temperature: 25°C.

[0033] Injection volume: 20 μL.

[0034] 3. Experimental steps

[0035] Weigh 5g of 2,4-dichloroacetophenone and 5g of o-methylacetophenone into a 100mL volumetric flask, dissolve and dilute to the mark with ethanol solution, and shake well. Obtain a sample solution.

[0036] 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. ...

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Abstract

The invention discloses a method for separating and determining 2,4-dichloroacetophenone and o-methylacetophenone 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 the mobile phaseis (80 to 60) to (20 to 40); 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 and the samplefeeding amount is 0.5 to 100muL; separation of 2,4-dichloroacetophenone and o-methylacetophenone is realized, and chromatographic conditions are provided for quantitative detection of the 2,4-dichloroacetophenone and the o-methylacetophenone.

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 o-methylacetophenone 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] Owing to can produce a certain amount of o-methyl acetophenone inevitably in the synthetic process of 2,4-dichloroacetophenone, the generation of o-methyl acetophenone has influenced the production of 2,4-dichloroacetophenone Purity, thereby affecting the synthetic effect of ketoconazole. [0004] The se...

Claims

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Application Information

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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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