Extract from indigo naturalis and a process for preparing the same

Patent metadata

Field	Value
Publication number	US-9861673-B2
Application number	US-201715592893-A
Country	US
Kind code	B2
Filing date	May 11, 2017
Priority date	Apr 9, 2015
Publication date	Jan 9, 2018
Grant date	Jan 9, 2018

Abstract

The present invention relates to a process for preparing an extract from one or more botanical raw materials, such as Indigo Naturalis and the extract itself. The present invention also relates to a composition comprising the extract, as well as the use of composition in medical or cosmetic applications.

First claim

The invention claimed is:

1. A process of preparing an extract product from Indigo Naturalis or a plant containing thereof, comprising:
a) extracting the Indigo Naturalis or the plant with a solvent to obtain a mixture of extraction, wherein the solvent is selected from the group consisting of dimethylformamide, ethyl acetate, ethanol, dimethylsulfoxide, dichloromethane, tetrahydrofuran, dimethylacetamide, acetone, 2-butanone, acetonitrile, isopropyl acetate, 2-methyl tetrahydrofuran, methyl tert-butyl ether, methanol, chloroform, terpene, water and a combination thereof,
b) filtering the mixture of extraction to obtain a filtrate,
c) concentrating the filtrate to obtain a crude extract,
d) mixing the crude extract with hexane or heptane at a temperature not less than 50° C. to obtain a washing mixture, and
e) filtering the washing mixture to obtain the extract product.

2. The process of claim 1 , wherein the solvent used in a) is selected from the group consisting of dimethylformamide, ethyl acetate, ethanol, and a combination thereof, or an aqueous solution thereof.

3. The process of claim 2 , wherein in e), the washing mixture is cooled and filtered at room temperature to obtain the extract product.

4. A process of preparing an extract product of Indigo Naturalis, comprising:
a) extracting the Indigo Naturalis with a solvent to obtain a mixture of extraction, wherein the solvent is selected from the group consisting of dimethylformamide, ethyl acetate, ethanol, dim ethyl sulfoxi de, dichloromethane, tetrahydrofuran, dim ethyl acetami de, acetone, 2-butanone, acetonitrile, isopropyl acetate, 2-methyl tetrahydrofuran, methyl tert-butyl ether, methanol, chloroform, terpene, water and a combination thereof,
b) filtering the mixture of extraction to obtain a filtrate,
c) concentrating the filtrate to obtain a crude extract,
d) mixing the crude extract and hexane or heptane in reflux to obtain a first washing mixture,
e) cooling and filtering the first washing mixture at room temperature obtain a first extract product, and
f) washing the first extract product with a washing method comprising:
i. mixing the first extract product and a solvent selected from the group consisting of hexane, ethanol and an aqueous solution of ethanol in reflux to obtain a second washing mixture, and
ii. cooling and filtering the second washing mixture at room temperature to obtain a second extract product.

5. The process of claim 4 , wherein in a), the solvent is selected from the group consisting of dimethylformamide, ethyl acetate, ethanol, and a combination thereof, or an aqueous solution thereof.

6. The process of claim 5 , wherein in a), the solvent is ethyl acetate, ethanol or an aqueous solution of ethanol, and the mixture of extraction is obtained by mixing the Indigo Naturalis and the solvent in reflux.

7. The process of claim 6 , wherein in b), the mixture of extraction is filtered at a temperature not less than 65° C. to obtain the filtrate.

8. The process of claim 7 , wherein prior to d), the crude extract is added with water and filtered to remove the solvent in the crude extract.

9. The process of claim 8 , wherein in d), the crude extract is mixed with hexane in reflux to obtain the first washing mixture.

10. The process of claim 9 , wherein the first extract product is rinsed with ethanol and water prior to f).

11. A process of preparing a refined extract comprising at least 55% (w/w) indirubin relative to the total weight of the refined extract, the process comprising:
a) extracting the Indigo Naturalis with a solvent to obtain a mixture of extraction, wherein the solvent is selected from the group consisting of ethyl acetate, ethanol, an aqueous solution of ethanol, and a combination thereof, and the mixture of extraction is obtained by mixing the Indigo Naturalis and the solvent in reflux,
b) filtering the mixture of extraction at a temperature of not less than 65° C. to obtain a filtrate,
c) concentrating the filtrate to obtain a crude extract,
d) mixing the crude extract and hexane in reflux to obtain a first washing mixture,
e) cooling and filtering the first washing mixture at room temperature to obtain a first extract product, and
f) washing the first extract product with a washing method comprising:
a) mixing the first extract product and a solvent selected from the group consisting of hexane, ethanol and an aqueous solution of ethanol in reflux to obtain a second washing mixture,
b) cooling and filtering the second washing mixture at room temperature to obtain a second extract product, and
c) drying the second extract product at a temperature of less than 80° C. to obtain a dried extract product,

g) optionally washing the dried extract product with the washing method of f) one or more times to thereby obtain the refined extract.

12. The process of claim 11 , further comprising micronizing the fine extract.

Assignees

• Galderma Sa

Inventors

• Lin Yin-Ku
• Cardinaud Isabelle
• Andres Philippe
• Chantalat Laurent
• Pierson Jean-Thomas
• Bily Antoine
• Le Bronec Loïc

Classifications

• A61P31/10

  Antimycotics · CPC title

• A61P29/00

  Non-central analgesic, antipyretic or antiinflammatory agents, e.g. antirheumatic agents; Non-steroidal antiinflammatory drugs [NSAID] · CPC title

• A61P35/00

  Antineoplastic agents · CPC title

• A61P17/12

  Keratolytics, e.g. wart or anti-corn preparations · CPC title

• A61P17/06

  Antipsoriatics · CPC title