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Method for preparing ketoside from gardenia

A technology of gardenia ketone glycosides and gardenia seeds, which is applied in the field of preparation of gardenia ketone glycosides, can solve problems such as low yield and complicated operation, and achieves the effects of simple operation, low energy consumption and easy industrial production.

Inactive Publication Date: 2013-12-04
NANJING BIAOKE BIO TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This type of method has the technical defects of complex operation and low yield

Method used

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  • Method for preparing ketoside from gardenia

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] Take 20kg of fresh gardenia jasminoides raw materials for beating, add 10 times the amount of 95% ethanol to fully stir, precipitate, filter the supernatant, add 5 times the amount of 95% ethanol solution to the filter residue and stir thoroughly, combine the two extracts to recover ethanol, concentrate Add water to dilute, then add hollow cellulose membrane with a molecular weight cut-off of 3000 for ultrafiltration, add HZ816 macroporous resin to the permeate for adsorption, first elute with 5 times the column volume of 20% ethanol solution, and then 10 times the volume of 60% ethanol solution. The eluate was then added to a hollow cellulose membrane with a molecular weight cut-off of 300 for nanofiltration, the collected concentrate was added to an equal volume of water-saturated n-butanol solution for extraction twice, and the extract was concentrated into an extract. Take ethyl acetate, n-butanol, and water, and mix them in a ratio of 1:2:4. Take the upper phase and...

Embodiment 2

[0020] Take 20kg of fresh gardenia jasminoides raw materials for beating, add 8 times the amount of 95% ethanol to fully stir, precipitate, filter the supernatant, add 7 times the amount of 95% ethanol solution to the filter residue and stir thoroughly, combine the two extracts to recover ethanol, concentrate Add water to dilute, add hollow cellulose membrane with a molecular weight cut-off of 3000 for ultrafiltration, and add ADS-21 macroporous resin to the permeate for adsorption. The eluate was then added to a hollow cellulose membrane with a molecular weight cut-off of 300 for nanofiltration, the concentrated solution was collected and added to an equal volume of water-saturated n-butanol solution for extraction three times, and the extract was concentrated into an extract. Take ethyl acetate, n-butanol, and water, and mix them in a ratio of 2:3:6. Take the upper phase and inject it into the chromatographic tube as the stationary phase. The speed of the host machine is 900 ...

Embodiment 3

[0022] Take 20kg of fresh gardenia jasminoides raw materials for beating, add 10 times the amount of 95% ethanol to fully stir, precipitate, filter the supernatant, add 3 times the amount of 95% ethanol solution to the filter residue and stir thoroughly, combine the two extracts to recover ethanol, concentrate After adding water to dilute, add hollow cellulose membrane with a molecular weight cut-off of 4000 for ultrafiltration, and add NK-9 macroporous resin to the permeate for adsorption. The eluate was then added to a hollow cellulose membrane with a molecular weight cut-off of 300 for nanofiltration, the concentrated solution was collected and added to an equal volume of water-saturated n-butanol solution for extraction three times, and the extract was concentrated into an extract. Take ethyl acetate, n-butanol, and water, and mix them in a ratio of 5:3:8. Take the upper phase and inject it into the chromatographic tube as the stationary phase. The main machine rotates at 8...

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Abstract

The invention discloses a method for preparing ketoside from gardenia. Operation for implementing the method is simple, and pollution caused during operation is low. The method includes steps of 1), mashing the fresh gardenia, adding 95% ethanol into the mashed fresh gardenia, sufficiently stirring the ethanol and the mashed fresh gardenia to obtain a mixture, depositing the mixture, performing suction filtration on the mixture to obtain supernatants, adding 95% of ethanol solution into filtration residues, sufficiently stirring the ethanol solution and the filtration residues, combining extracting solution obtained in two extracting procedures to recycle ethanol, adding an appropriate amount of water into concentrated solution to dilute the concentrated solution, adding the diluted concentrated solution into an ultrafiltration membrane, performing ultrafiltration on the diluted concentrated solution, adding permeate solution into macro-porous resin columns, performing adsorption on the permeate solution, eluting the permeate solution by the aid of ethanol solution in a gradient manner, performing nano-filtration on eluent by the aid of a nano-filtration membrane and collecting concentrated solution; 2), adding water-saturated n-butyl alcohol into the concentrated solution to extract the concentrated solution, collecting extracting solution, concentrating the extracting solution under a vacuum condition, separating the concentrated solution by means of high-speed countercurrent chromatography, collecting fractions according to a chromatogram, drying the fractions under a vacuum condition to obtain the ketoside. The quantity of the 95% ethanol added into the fresh mashed gardenia is 3-10 times that of the mashed fresh gardenia. The method has the advantages that the operability is high, and the method is suitable for preparing high-purity ketoside from gardenia.

Description

technical field [0001] The invention belongs to the field of biotechnology, in particular to a preparation method of geniposide. Background technique [0002] Geniposide belongs to iridoid glycosides, CAS No. 54835-76-6, molecular formula C16H22O10, molecular weight 374.35, molecular structural formula: [0003] [0004] Gardenia jasminoides, also known as jasmine jasmine, shanzhi, and white toad, is the fruit of the Rubiaceae plant gardenia, containing flavonoids gardenia, pectin, tannin, saffron, saffron acid, D-mannitol, 29 Alkanes, β-sitosterol, geniposide, geniposide and shangenin B and other components have the effects of purging fire and eliminating troubles, clearing heat and dampness, cooling blood and detoxification, and are used to treat cardiovascular and cerebrovascular diseases, liver and gallbladder and other diseases. [0005] Through literature search, the existing preparation methods of geniposide mostly adopt silica gel column separation. This type o...

Claims

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Application Information

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IPC IPC(8): C07D407/12
Inventor 张金芳万冬梅
Owner NANJING BIAOKE BIO TECH