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A high-content natural shikimic acid extract product and a preparing method thereof

A technology of shikimic acid and extract, applied in the field of separation and preparation of shikimic acid extract, can solve problems such as environmental pollution, producer, environmental impact, and film blockage, and achieves alleviation of plant resource shortage problems, low requirements for instruments and equipment, and low operation requirements. simple effect

Active Publication Date: 2017-11-17
YUNNAN HIKON BIOTECH CO LTD +2
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In addition, the extraction of shikimic acid from star anise, etc. is often applied to toxic reagents such as acetone and chloroform, which will have a certain impact on producers and the environment.
For example, in the method disclosed in "A Process for Simultaneously Extracting Shikimic Acid and Essential Oils from Star Anise" (Patent Application No. 200610126418.2), star anise is extracted with water, the water extract is concentrated to obtain a syrup, and the syrup is extracted with acetone. The acetone extract is dried to obtain crude shikimic acid, and then the crude product is adsorbed on silica gel-methanol-chloroform elution and recrystallized to obtain fine shikimic acid. In the process, a large amount of organic reagents such as acetone and chloroform are used, which is difficult to recover. pollute the environment
In the method disclosed in "A Preparation Method of Shikimic Acid" (Patent Application No. 200910234064.7), star anise is extracted with water, the water extract containing shikimic acid is separated by membrane to remove macromolecular substances such as protein and polysaccharide, and ion exchange resin is used to adsorb and separate , and finally methanol recrystallization to obtain fine shikimic acid, but membrane separation technology can only remove macromolecular substances, and it is easy to cause membrane blockage and pollution

Method used

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  • A high-content natural shikimic acid extract product and a preparing method thereof
  • A high-content natural shikimic acid extract product and a preparing method thereof
  • A high-content natural shikimic acid extract product and a preparing method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] Example 1: Content detection of shikimic acid in ginkgo biloba and production wastewater

[0029] The method for determining the content of shikimic acid in Ginkgo biloba and macroporous resin washing liquid is as follows:

[0030] Instrument: Agilent HPLC 1260

[0031] Stationary phase: Agilent XDB-C8 column 250mm×4.6mm, 5μm

[0032] Table 1 mobile phase and gradient list

[0033]

[0034] Flow rate: 1.0ml / min; detection wavelength: 215nm; injection volume: 10μL.

[0035] The results are shown in Table 2. The content of shikimic acid in Ginkgo biloba is basically 3-5%, and most of the shikimic acid is finally lost through the macroporous resin step.

[0036] Table 2 Shikimic acid detection results

[0037]

[0038] Note: The feeding amount of ginkgo biloba for each batch is 1 ton.

Embodiment 2

[0039] Embodiment 2: the selection of purification resin

[0040] Take ginkgo biloba extract production waste water, use D941, D315, D290, D201, D296, 201*7 type anion exchange resin to absorb and separate, first wash with water, and then use aqueous solution containing 1mol / L NaOH to obtain the eluate After concentration and drying, the transfer rate of shikimic acid and the content of shikimic acid in the extract were determined.

[0041]The results are shown in Table 3. D941 anion exchange resin has the highest transfer rate of shikimic acid. Although D315 anion exchange resin has the highest content of shikimic acid in the purified extract, the transfer rate is less than 40%. Therefore, D941 anion exchange resin was selected for adsorption separation.

[0042] Table 3 Anion exchange resin type screening

[0043]

Embodiment 3

[0044] Example 3: Screening of Elution and Impurity Removal Solvents

[0045] Take ginkgo biloba extract production wastewater, use D941 anion exchange resin to absorb and separate, wash with water, and then sequentially elute with aqueous solution containing 0.01, 0.1 and 1mol / L HCl, collect each eluted part, concentrate and dry, and measure the transfer of shikimic acid rate and content; or wash with water first, and then sequentially elute with an aqueous solution containing 0.005, 0.025, 0.05, 0.1, 0.5, 1mol / L NaOH, collect each eluted part, concentrate and dry, and measure the transfer rate and content of shikimic acid.

[0046] The results are shown in Table 4. After being eluted with an aqueous solution containing HCl, the color of the concentrated solution gradually deepened during the concentration process, and finally turned black. It may be that under strong acidic conditions, both sugar and shikimic acid were dehydrated and carbonized, making the content of shikimic...

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Abstract

The invention discloses a high-content natural shikimic acid extract product separated and prepared from waste water generated in a ginkgo leaf extract product production process and a preparing method thereof. The content of shikimic acid is higher than 98%. The waste water generated in the ginkgo leaf extract product production process is adopted as a raw material of the method, and the method includes directly subjecting the waste water to adsorption separation with anion exchange resin, allowing the eluate obtained to pass through cation exchange resin to remove sodium, subjecting a solution after sodium removal to three combined steps of adding a shikimic acid high-purity product, performing high-temperature treatment, and allowing the mixture to stand at a low temperature in order to precipitate a shikimic acid precipitate, and recrystallizing the shikimic acid precipitate to obtain the shikimic acid extract product the shikimic acid content of which is 98% or above.

Description

technical field [0001] The invention relates to natural plant extracts, in particular to a method for separating and preparing shikimic acid extracts from ginkgo biloba extract production wastewater. Background technique [0002] Ginkgo biloba and its extracts are rich in organic acids. For example, the content of organic acids in Ginkgo standard extract EGb761 reaches 13%. These organic acids include shikimic acid, protocatechuic acid, p-hydroxybenzoic acid, gallic acid, etc. [0003] The chemical name of shikimic acid is 3,4,5-trihydroxy-1-cyclohexyl-1-carboxylic acid, and the molecular formula is C 7 h 10 o 5 , is a common small molecule organic acid, easily soluble in water, the solubility in water is 18g / 100ml. Shikimic acid is the key precursor of many important compounds, such as alkaloids, aryl amino acids and chiral drug synthesis, and it is also the starting material for the synthesis of anti-avian influenza drug - Tamiflu. At present, there are three main sour...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C62/32C07C51/42C07C51/47C07C51/43
CPCC07C51/42C07C51/43C07C51/47C07C62/32
Inventor 乔洪翔陈君王如伟黄海波吴华铃金朱明陈国俊方玲陈岑张云飞
Owner YUNNAN HIKON BIOTECH CO LTD
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