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Method for preparing high-purity crocetin with gardenia yellow pigment

A technology of gardenia yellow pigment and crocetin, applied in the field of new medicine, can solve problems such as large environmental pollution, toxicity of chemical reagents, and failure to meet quality indicators, achieve high product content, overcome difficulty in extraction, and avoid process complex effects

Inactive Publication Date: 2015-03-11
WEIHAI NOVODA PHARMA GRP
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The purpose of the present invention is to solve the problems that the purity of the crocetin extracted and prepared in the prior art is not high, the quality index does not reach the standard of the pharmaceutical industry, the chemical reagents used in the technology are more toxic, the environment is polluted, and the production cost is high. Extract and separate gardenia yellow pigment with silica gel chromatography to obtain crocin with high purity, and then carry out alkaline hydrolysis on crocin to obtain crocetin with a purity of more than 90%. The method used to separate crocin is Silica gel column chromatography, crocin hydrolysis adopts alkaline hydrolysis method

Method used

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  • Method for preparing high-purity crocetin with gardenia yellow pigment

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Experimental program
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Effect test

Embodiment 1

[0031] 1. Isolation of crocin

[0032] (1) Preparation: Mix the silica gel and ethyl acetate thoroughly, soak for 12 hours, set aside, take an appropriate amount of gardenia yellow pigment

[0033] solution, add water to make a paste, dry at 50°C, grind into powder, and set aside, use ethyl acetate:methanol:water at a ratio of 10:2:1 as the mobile phase for silica gel chromatography;

[0034] (2) Dissolution: Take 0.5 g of refined gardenia yellow pigment and dissolve it in 95% methanol;

[0035] (3) Column loading: take 1 g of 200-300 mesh column chromatography silica gel, slowly add the dissolving solution in step (2) into the silica gel, stir while adding, mix thoroughly, and then evaporate the methanol at a low temperature of 40°C Dry, take 100 g of 200-300 mesh column chromatography silica gel, mix the mobile phase with the silica gel in (1), put it into the packed column, and slowly add the column chromatography silica gel mixed with gardenia yellow pigment essence into ...

Embodiment 2

[0051] 1. Isolation of crocin

[0052] (1) Preparation: Mix the silica gel and ethyl acetate thoroughly, soak for 12 hours, set aside, take an appropriate amount of gardenia yellow pigment

[0053] solution, add water to make a paste, dry at 50°C, grind into powder, set aside, use ethyl acetate:methanol:water 15:4:2 solution as the mobile phase for silica gel chromatography;

[0054] (2) Dissolution: Take 0.5 g of refined gardenia yellow pigment and dissolve it in 95% methanol;

[0055] (3) Column loading: take 1 g of 200-300 mesh column chromatography silica gel, slowly add the dissolving solution in step (2) into the silica gel, stir while adding, mix thoroughly, and then evaporate the methanol at a low temperature of 40°C Dry, take 100 g of 200-300 mesh column chromatography silica gel, mix the mobile phase with the silica gel in (1), put it into the packed column, and slowly add the column chromatography silica gel mixed with gardenia yellow pigment essence into the chrom...

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Abstract

The invention discloses a method for preparing high-purity crocetin with a gardenia yellow pigment. The method comprises the steps of extracting and separating the gardenia yellow pigment by silicagel column chromatography to form crocin with higher purity, hydrolyzing crocin under an alkaline condition to form crocetin with the higher purity. After the gardenia yellow pigment is separated and eluted by a chromatographic column, an eluant is collected and dried; a crocin content can reach above 90% through detection under 440nm wavelength of high efficiency liquid chromatography; after alkaline hydrolysis and N,N-dimethylformamide recrystallization, the purity of crocetin can reach above 95% through detection under 420nm wavelength of the high efficiency liquid chromatography; the prepared product is high in purity; the technology operability is strong; and the method can be widely applied to the field of medicines.

Description

technical field [0001] The invention relates to a method for preparing high-purity crocetin, that is, a method for preparing crocetin by using crocetin in gardenia yellow pigment as a substrate, and belongs to the field of new medicines. Background technique [0002] Studies have shown that saffron has good anti-tumor activity, and has various pharmacological effects such as anti-virus, anti-oxidation, anti-coagulation and immune regulation. Crocetin acid is one of the main active components in saffron, which has obvious The anti-atherosclerotic effect of saffron, but as a precious medicinal material, my country still mainly relies on imports for medicinal purposes. Although it has been introduced and cultivated to provide a small amount of commodities, due to the lack of provenance, limited areas suitable for cultivation, and harsh conditions, etc. Factors, can not meet the needs of the market, there has been a situation of short supply. [0003] In order to solve this situa...

Claims

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Application Information

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IPC IPC(8): C07C57/13C07C51/09C07C27/02C07C51/42C07H13/06C07H1/08
CPCC07C51/09C07C1/08C07C51/42C07H13/06
Inventor 王河东李磊
Owner WEIHAI NOVODA PHARMA GRP
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