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Method for preparing high-purity geniposide

A high-purity technology of geniposide, applied in the field of preparation of high-purity geniposide, can solve the problems of unfavorable industrial production, complex process, unfavorable separation, etc., and achieve the effects of improved separation effect, high product yield and short production cycle

Inactive Publication Date: 2012-04-04
GUANGXI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] The separation methods of geniposide in Gardenia mainly include silica gel column chromatography, macroporous resin adsorption, two-phase extraction, extraction under alkaline conditions, ultrafiltration membrane separation, supercritical CO 2 Fluid extraction, high-speed countercurrent chromatography, etc., these methods have certain shortcomings and are not conducive to industrial production
Its main problems are: complex process, excessive material consumption, low yield, and the use of toxic and harmful reagents in large quantities, such as ether, chloroform, methanol, acetone, etc.; adding a large amount of salt and alkali to extract geniposide, under alkaline conditions The glycosides may be hydrolyzed, and other acidic substances are not conducive to separation after deterioration

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0035] Weigh 500g of gardenia fruit coarse powder, add 2500ml mass concentration of 75% ethanol aqueous solution, ultrasonically extract 4 times at 30°C, extract for 1 hour each time, combine 4 extracts and concentrate under reduced pressure to obtain a 20% mass concentration extractum, Extract continuously 4 times with equal-volume ethyl acetate, collect the lower-phase aqueous solution that obtains, get 200.0g lower-phase aqueous solution and add 0.75g carboxymethyl cellulose sodium to fully dissolve, then use n-butanol of mixed solution equal volume: acetic acid Ethyl ester volume ratio is 1: 1 mixed solvent extraction 3 times, combine the upper phase solution of 3 extractions, decolorize with activated carbon, concentrate under reduced pressure to obtain 8.0g of geniposide crude product, the crude product is 80% ethanol aqueous solution at room temperature condition 5.6 g of geniposide crystals can be obtained by recrystallization under low pressure, the purity is 91.0%, an...

Embodiment 2

[0037] Weigh 500g of gardenia fruit coarse powder, add 2500ml of aqueous solution, and ultrasonically extract 4 times at 50°C for 1 hour each time. After ethyl acetate was extracted continuously for 4 times, the lower phase aqueous solution obtained was collected, and 200.0 g of the lower phase aqueous solution was taken, and after adding 2.5 g of molecular weight, polyethylene glycol with a molecular weight of 2000 was fully dissolved, and then mixed solution with n-butanol of equal volume: ethyl acetate The volume ratio of the ester was 1:1 and the mixed solvent was extracted 3 times, the upper phase solutions of the 3 extractions were combined, decolorized with activated carbon, and concentrated under reduced pressure to obtain 3.9 g of geniposide crude product. The crude product was 80% ethanol aqueous solution at room temperature. 3.1 g of geniposide crystals can be obtained by recrystallization, the purity is 98.0%, and the yield of geniposide is 62.0%.

Embodiment 3

[0039] Weigh 500g of gardenia fruit coarse powder, add 3500ml mass concentration of 75% ethanol aqueous solution, ultrasonically extract 4 times at 40°C, extract for 1 hour each time, combine 4 extracts and concentrate under reduced pressure to obtain 20% mass concentration extractum, Continuously extract the medicinal extract 4 times with an equal volume of ethyl acetate, take 245.0 g of the lower phase aqueous solution, add 2.5 g of polyacrylamide into the lower phase aqueous solution to fully dissolve, and then use an equal volume of n-butanol in the mixed solution: ethyl acetate volume The mixed solvent with a ratio of 1:1 was extracted 4 times, the upper phase solutions of the 4 extractions were combined, decolorized with activated carbon, and concentrated under reduced pressure to obtain 8.2 g of crude geniposide, which was recrystallized with 80% ethanol aqueous solution at room temperature 6.4 g of geniposide crystals can be obtained, the purity of which is 96.0%, and t...

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Abstract

The invention discloses a method for preparing high-purity geniposide. The method comprises the following steps of: extracting active ingredients from gardenia fruits by using a 75 mass percent ethanol aqueous solution or water under the ultrasonic wave condition; extracting extractum obtained after concentration by using ethyl acetate; adding polymers such as sodium carboxymethylcellulose, polyacrylamide, polyethylene glycol and the like into a retained bottom phase aqueous solution and dissolving completely; extracting by using a mixed solvent of normal butanol and ethyl acetate; merging an upper phase organic solution; decoloring by using active carbon; concentrating under reduced pressure and performing vacuum drying to obtain a geniposide crude product; and recrystallizing the geniposide crude product to obtain the high-purity geniposide. The method is easy to operate; the production cycle is short; yield and purity of the products are high; and the method is suitable for industrialized mass production.

Description

technical field [0001] The invention belongs to the technical field of extracting active ingredients from plants. Specifically, it is a method for preparing high-purity geniposide. technical background [0002] Gardenia is the dry and mature fruit of Gardenia jasminoides of the Rubiaceae family. Its shape is pointed and oblong, and the outer skin is ribbed. Gardenia is divided into mountain gardenia and water gardenia. The main producing areas of gardenia in my country are Zhejiang, Jiangxi, Fujian, Anhui, Hunan, Taiwan and other places. Gardenia has the effects of purging fire and relieving restlessness, clearing heat and dampness, cooling blood and detoxifying, etc. It is used clinically to treat hypertension, sprains, diabetes, high fever jaundice, and short red urine. The chemical components of Gardenia are mainly iridoids, triterpenes, flavonoids, crocin, organic acids and volatile oils. Geniposide is one of the iridoids in Gardenia jasminoides. It has various pharma...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07H17/04C07H1/08
Inventor 韦万兴唐新宗周敏凌秀荣
Owner GUANGXI UNIV
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