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Method for extracting crocetin from gardenia

A technology of crocetin and gardenia, which is applied in the field of extraction and preparation of crocetin, and can solve problems such as the difficulty of crocetin

Active Publication Date: 2008-07-23
INST OF PROCESS ENG CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The types and contents of crocetin contained in saffron and gardenia are different, but after hydrolysis, only trans and cis crocetin are obtained, and because crocetin is insoluble in water, it is easy to mix with other ingredients separate

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0011] 1) Crush the dried gardenia fruit, pass a 20-mesh sieve, add 15 times the amount of 50% ethanol solution to the gardenia powder, and ultrasonically extract at 25°C for 40 minutes, with a power of 50W / cm 2 , The extract is filtered, the residue is added with 8 times the amount of ethanol solution, and then extracted for 20 minutes, the extract is filtered, combined, vacuum concentrated to remove the ethanol, the concentrated solution is diluted with water to A 440nm For 1000, filter with suction and take the clear filtrate;

[0012] 2) Add 2M KOH solution to the crocin clear liquid of step 1), adjust the pH to 13, and let stand for 6 hours at 20°C, then adjust the pH to 4.5 with 2M hydrochloric acid solution, centrifuge at 5000rpm for 20min, discard the supernatant, and take Precipitate, add water to wash 2-3 times, centrifuge as above to get the precipitate, it is crude crocetic acid, the purity is about 90%;

[0013] 3) The crude crocetin in step 2) is dissolved in methano...

Embodiment 2

[0015] 1) Crush the dried gardenia fruit, pass a 40-mesh sieve, add 20 times the amount of 30% ethanol solution to the gardenia powder, and ultrasonically extract at 25°C for 10 minutes, with a power of 80W / cm 2 , The extract is filtered, the residue is added with 10 times the amount of 30% ethanol solution, and then extracted for 10 minutes, the extract is filtered, combined, vacuum concentrated to remove the ethanol, the concentrated solution is diluted with water to A 440nm 250-500, suction filtration, take the clear filtrate;

[0016] 2) The above clarified filtrate is added to the ADS-7 macroporous resin column, the column diameter-to-height ratio is 1:15, and the sample volume is 1:1 to the column bed volume. Wash with water and 20% ethanol solution 4 times the column bed volume. Remove, collect the eluate, concentrate to obtain the crude geniposide, and then eluted with 50% and 75% ethanol, each 5 times the volume of the column bed, the eluate was concentrated to remove the...

Embodiment 3

[0020] 1) Crush the dried gardenia fruit, pass through a 60-mesh sieve, add 20 times the amount of 80% ethanol solution to the gardenia powder, and ultrasonically extract at 25°C for 30 minutes, with a power of 30W / cm 2 , The extract is filtered, concentrated in vacuo to remove ethanol, and the concentrate is diluted with water to A 440nm 500, suction filtration, take clear filtrate;

[0021] 2) Add 2M KOH solution to the clarified filtrate of crocin in step 2), adjust the pH to 14, and let stand at 50°C for 0.5h, then adjust the pH to 4.5 with 1M hydrochloric acid solution, centrifuge at 5000rpm for 20min, and discard the supernatant. Take the precipitate, wash it 2-3 times with water, and centrifuge the precipitate as above to obtain the crude crocetic acid with a purity of about 90%;

[0022] 3) The crude crocetin in step 3) is dissolved in methanol, 0.5M acetic acid solution is added to make 1 / 4 of the methanol, the precipitated precipitate is centrifuged at 5000rpm for 20min,...

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Abstract

The invention relates to a preparation method of the crocetin extracted from the gardenia, which is characterized in that after the gardenia is crushed and extracted by ultrasonic enhancement in distilled water or ethanol solution, the extractant is filtered and concentrated; the glycoside substance of the gardenia is separated via the macroporous resin and the crocin eluent is concentrated and dealt with acid hydrolysis or alkaline hydrolysis (alkaline hydrolysis solution should be adjusted to pH of acidity.), centrifugal, rinse and sedimentation to get the crude product of the crocetin; after purifying the crude product of the crocetin further, the cis crocetin and the trans crocetin are separated to acquire trans crocetin of high purity which facilitates structure modification, forms a plurality of crocetin derivatives featured by different water soluble and drug efficacy, providing material for related preparation R and D and application. The preparation method of the crocetin extracted from the gardenia has the advantages of having convenient and fast method, low cost and establishing a new channel for deep processing of gardenia products.

Description

Technical field [0001] The invention relates to a method for extracting and preparing crocetic acid from gardenia. Background technique [0002] Gardenia is the dry mature fruit of the Rubiaceae plant Gardenia. It is mainly produced in Jiangxi, Hunan, Guangxi, Sichuan and other places. The common cultivated varieties are: Gardenia (Gardeniajasminodes Ellis), which is a pharmacopoeia specified variety; Water Gardenia (G .jasminodesEllis f.longiarpa ZWXie et Okada), a variant of gardenia, used as dyes and pigments; gardenia (double-petaled gardenia) (G.jasminodes Ellis var.fortuniana (Lind1) Ham), of gardenia Varieties, garden cultivation. At present, in addition to its application in traditional Chinese medicine, gardenia is mainly used as a raw material for extracting natural pigments for the preparation of gardenia, gardenia red, and gardenia yellow pigments. Among them, the main component of gardenia yellow pigment is crocin (Nasha, Guo Tianguo. Progress in pharmacological rese...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C57/13C07C51/42A61K36/744A61P35/00A61P9/00
Inventor 赵兵陈文浩王玉春王晓东
Owner INST OF PROCESS ENG CHINESE ACAD OF SCI
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