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Method for detecting related substances of 6-chloro-2-hexanone

A technology related to substances and detection methods, applied in the field of analytical chemistry, to achieve good recovery and stability, good separation, and accurate and reliable detection results

Active Publication Date: 2021-10-01
沧州临港友谊化工有限公司
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] Aiming at the absence of a detection method for related substances of 6-chloro-2-hexanone at present, the present invention provides a detection method for related substances of 6-chloro-2-hexanone, thereby improving The quality stability and clinical drug safety of pentoxifylline synthesized from raw materials

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  • Method for detecting related substances of 6-chloro-2-hexanone
  • Method for detecting related substances of 6-chloro-2-hexanone
  • Method for detecting related substances of 6-chloro-2-hexanone

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Embodiment 1

[0032] This embodiment provides a method for detecting related substances of 6-chloro-2-hexanone, the steps are as follows:

[0033] 1.1 Solution preparation

[0034] Preparation of the test solution: Accurately weigh an appropriate amount of 6-chloro-2-hexanone, add dichloromethane to dissolve and dilute to a solution containing 20 mg of 6-chloro-2-hexanone per 1 mL, and obtain the solution.

[0035] Preparation of mixed reference solution: Accurately weigh 5-hexen-2-one, bromochloropropane, ethyl acetoacetate, 3-chloro-1-propanol, 5,6-dihydro-3-ethoxycarbonyl -2-Methyl-4H-pyran, 6-caprolactone-2-one appropriate amount of reference substance, respectively dissolved and diluted with dichloromethane, mixed until each 1mL contains about 20μg of 5-hexen-2-one, Bromochloropropane 20 μg, ethyl acetoacetate 20 μg, 3-chloro-1-propanol 80 μg, 5,6-dihydro-3-ethoxycarbonyl-2-methyl-4H-pyran (INT1) 20 μg, 6- A mixed solution of 80 μg of caprolactone-2-one was obtained.

[0036] Prepar...

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Abstract

The invention relates to the field of analytical chemistry, in particular to a method for detecting related substances of 6-chloro-2-hexanone. The detection method adopts a gas chromatographic method for determination, and chromatographic conditions are as follows: a stationary liquid of a capillary chromatographic column is polyethylene glycol or modified polyethylene glycol; and in a heating procedure, the initial temperature is 45-55 DEG C, the temperature is increased to 220-240 DEG C at the speed of 5-15 DEG C / min, and the temperature is maintained for 5-10 min. The detection method provided by the invention is good in sensitivity, accuracy, precision, reproducibility, recovery rate and stability, and accurate and reliable in detection result, and provides a guarantee for monitoring the quality stability and clinical medication safety of pentoxifylline synthesized by taking 6-chloro-2-hexanone as a starting material.

Description

technical field [0001] The invention relates to the field of analytical chemistry, in particular to a method for detecting related substances of 6-chloro-2-hexanone. Background technique [0002] Pentoxifylline is a non-selective phosphodiesterase inhibitor. By inhibiting phosphodiesterase, it increases intracellular adenosine triphosphate, improves the deformability of red blood cells, reduces fibrinogen, and inhibits the aggregation of red blood cells and platelets. As a non-specific peripheral vasodilator, pentoxifylline can relax the isolated canine basilar artery, enhance the deformability of red blood cells in rats, and increase the oxygen-carrying capacity of tissues; reduce blood viscosity and increase capillary flow, thereby improving blood fluidity and promoting blood circulation. The microcirculation of ischemic tissue can increase the oxygen supply of special organs, and its metabolites can also improve blood viscosity and microcirculation. [0003] 6-Chloro-2-h...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02G01N30/06G01N30/86
CPCG01N30/02G01N30/06G01N30/8634
Inventor 杨俊免宗莹莹陈碧楚王亚静董海峰张龙梅徐黎明楚梦茹李彤周雅洁牛若凡
Owner 沧州临港友谊化工有限公司
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