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A kind of etodolac photodegradation impurity and preparation method thereof

A technology of etodolac and impurities, applied in the field of etodolac photodegradation of impurities and its preparation, can solve problems such as not given, and achieve the effects of preventing sample re-degradation, strong pertinence, and simple and fast processing methods

Active Publication Date: 2020-08-21
LUNAN PHARMA GROUP CORPORATION
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] Xu Meiju et al. (high performance liquid chromatography to measure the content of etodolac, Guangdong Chemical Industry, 2013, 40, (5) 19-23) disclose that etodolac is subjected to acid destruction, alkali destruction, oxidation destruction, light destruction and heat destruction respectively. Destruction test, and detect the components after the destruction test, and obtain the high performance liquid chromatogram after the destruction test, but do not give the corresponding impurity items

Method used

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  • A kind of etodolac photodegradation impurity and preparation method thereof
  • A kind of etodolac photodegradation impurity and preparation method thereof
  • A kind of etodolac photodegradation impurity and preparation method thereof

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Experimental program
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Effect test

Embodiment 1

[0065] Embodiment 1: the preparation of formula I impurity compound

[0066] Dissolve the etodolac sample in acetonitrile, prepare 100ml of 10mg / ml acetonitrile solution, add 1ml of hydrogen peroxide solution with a mass fraction of 3%, and mix well to obtain the etodolac solution to be destroyed; place the above etodolac solution to be destroyed In the light destruction box, set the temperature at 20°C, light intensity 5000Lx, and carry out light destruction for 15 hours to obtain etodolac light destruction liquid; sample for HPLC detection, the HPLC purity of the impurity compound of formula I is 60.91%.

Embodiment 2

[0067] Embodiment 2: the preparation of formula I impurity compound

[0068] Dissolve the etodolac sample in tetrahydrofuran, prepare 100ml of 15mg / ml tetrahydrofuran solution, add 5ml of hydrogen peroxide solution with a mass fraction of 1%, and mix well to obtain the etodolac solution to be destroyed; place the above etodolac solution to be destroyed In the light destruction box, set the temperature at 30° C., light intensity 3000Lx, and carry out light destruction for 20 hours to obtain etodolac light destruction liquid; take samples for HPLC detection, and the HPLC purity of the impurity compound of formula I is 57.45%.

Embodiment 3

[0069] Embodiment 3: the preparation of formula I impurity compound

[0070] Dissolve the etodolac sample in ethyl acetate, prepare 100ml of 10mg / ml ethyl acetate solution, add 0.5ml of hydrogen peroxide solution with a mass fraction of 5%, and mix to obtain etodolac solution to be destroyed; The acid-to-be-destroyed solution was placed in a light-destroyed box, set at a temperature of 25° C., and subjected to light-destroyed 10 hours with a light intensity of 6000 Lx to obtain etodolac light-destroyed solution; samples were taken for HPLC detection, and the HPLC purity of the impurity compound of formula I was 55.65%.

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Abstract

The invention belongs to the field of biological medicines and specifically relates to an etodolic acid photodegradation impurity and a preparation method thereof. The preparation method comprises thesteps: dissolving etodolic acid into an organic solvent; carrying out illumination damage under an aerobic condition; and carrying out supercritical fluid chromatographic separation and purificationto obtain the etodolic acid photodegradation impurity with high purity. The total yield of the etodolic acid photodegradation impurity obtained by using the preparation method exceeds 48%, the supercritical fluid chromatographic purification yield exceeds 90%, and the purity of the obtained etodolic acid photodegradation impurity reaches up to 99.01%.

Description

technical field [0001] The invention belongs to the field of biomedicine, and in particular relates to an etodolac photodegradation impurity and a preparation method thereof. Background technique [0002] [0003] Etodolac is a pyranose carboxylic acid steroid anti-inflammatory drug, which inhibits the synthesis of prostaglandin (PG) by blocking the activity of cyclooxygenase, and has anti-inflammatory, antipyretic and pain-relieving effects. It is clinically used to treat postoperative pain and relieve the symptoms of rheumatoid arthritis and osteoarthritis. At the same time, the widespread use of drugs has become an emerging environmental pollution factor. It is very necessary to study and control various impurity items in pharmaceutical production. [0004] Xu Meiju et al. (high performance liquid chromatography to measure the content of etodolac, Guangdong Chemical Industry, 2013, 40, (5) 19-23) disclose that etodolac is subjected to acid destruction, alkali destruc...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D267/00
CPCC07D267/00Y02P20/54
Inventor 张贵民郝大伟刘东
Owner LUNAN PHARMA GROUP CORPORATION