Method for determining 2,4-dichloroacetophenone and 2,6-dichloroacetophenone isomers through gas chromatographic separation

A technology of dichloroacetophenone and gas chromatography, which is applied in the directions of material separation, measurement device, analysis material, etc., can solve the problems such as separation and measurement that have not been reported in the literature.

Active 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 determining 2,4-dichloroacetophenone and 2,6-dichloroacetophenone isomers through gas chromatographic separation
  • Method for determining 2,4-dichloroacetophenone and 2,6-dichloroacetophenone isomers through gas chromatographic separation
  • Method for determining 2,4-dichloroacetophenone and 2,6-dichloroacetophenone isomers through gas chromatographic separation

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Embodiment 1

[0027] 1. Instrument

[0028] Gas chromatograph: Shimadzu, GC-2014AT, hydrogen flame detector.

[0029] Chromatographic column: HP-5 (30m×0.32mm×0.5μm).

[0030] 2. Chromatographic conditions

[0031] Carrier gas: nitrogen

[0032] Flow rate: 1.0 mL / min.

[0033] Detector: hydrogen flame detector.

[0034] Injector temperature: 250°C.

[0035] Detector temperature: 280°C.

[0036] Column temperature: 170°C.

[0037] Injection volume: 2 μL.

[0038] Using constant temperature separation.

[0039] 3. Experimental steps

[0040] 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 to obtain a sample solution.

[0041] Take 2 μL of the above solution, analyze according to the above chromatographic conditions, and record the chromatogram, the results are as follows: figure 1 shown.

[0042] figure 1 The chromatographic peak with a retention value of 4...

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Abstract

The invention discloses a method for determining 2,4-dichloroacetophenone and 2,6-dichloroacetophenone isomers through gas chromatographic separation. According to the method, an HP-5 weak-polarity capillary column is adopted and has the specification of 30m*0.32mm*0.5mu m; carrier gas is nitrogen gas and the flow speed of the carrier gas is 1.0mL/min; a hydrogen flame detector is adopted; the temperature of a sample feeding opening of a gas chromatograph is 200 to 280 DEG C, the temperature of a column box is 130 to 180 DEG C and the temperature of the detector is 250 to 300 DEG C; constant-temperature separation is carried out and the sample feeding amount is 2mu L; finally, separation of 2,4-dichloroacetophenone and 2,6-dichloroacetophenone is realized; chromatographic conditions are provided for quantitative detection of 2,4-dichloroacetophenone and 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 gas 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 separation and identifi...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/68G01N30/06
CPCG01N30/06G01N30/68
Inventor 陈舟
Owner 常州市盛辉药业有限公司
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