Method for extracting syringin

A technology of syringin and thermal insulation extraction, which is applied in chemical instruments and methods, preparation of sugar derivatives, sugar derivatives, etc., can solve the problems of low content of raw materials, complicated process and high cost, and achieves high content, simple operation and high cost. low effect

Inactive Publication Date: 2011-05-25
NANJING ZELANG MEDICAL TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] As mentioned above, there are problems in the existing methods: extracting from Acanthopanax, Saussurea and white clove, the raw material content is low, resulting in complicate

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Example Embodiment

[0019] Example 1:

[0020] Crush the raw holly 20 mesh, take 1kg, add 15kg of water and heat to 80℃, keep for 3 hours, extract the extract, add 8kg of water and keep at 80℃ for 2 hours, filter out the extract, add 6kg of water to keep at 80℃ For 2 hours, combine the three extracts and concentrate to 100ml under reduced pressure. Add 1L of 95% ethanol to the concentrate to azeotrope, then add 20g of medicinal activated carbon to decolorize, adjust the pH to 3 with hydrochloric acid of the decolorized liquid, place the precipitate, filter impurities, and adjust the filtrate with sodium hydroxide solution. Concentrate under reduced pressure until alcohol-free, add 100ml of water saturated n-butanol to extract 4 times, collect the n-butanol extract layer, recover the n-butanol under reduced pressure, add appropriate amount of water to stand for crystallization, obtain 32g of crystals, add 300ml of water to reflux for crystallization, The crystals were filtered out and then dissolved ...

Example Embodiment

[0021] Example 2:

[0022] Crush 60 mesh iron holly raw material, take 1kg, add 20kg of water and heat to 70℃, keep for 3 hours, extract the extract, add 10kg of water and keep for 2 hours at 70℃, combine the extract and concentrate to 150ml under reduced pressure, add the concentrated solution 1.5L 90% ethanol azeotrope, then add 30g medicinal activated carbon to decolorize, adjust pH1 of decolorizing liquid phosphoric acid, place the precipitate, filter impurities, adjust the filtrate with potassium hydroxide solution to neutralize and concentrate under reduced pressure to alcohol-free, add 150ml water saturated n-butanol Extract 3 times, collect the n-butanol extract layer, recover the n-butanol under reduced pressure, add an appropriate amount of water to crystallize to obtain 38g of crystals, add 400ml of water to reflux for crystallization, filter out the crystals and reflux with 60% acetone solution to dissolve, filter The crystals were placed, and the crystals were dried ...

Example Embodiment

[0023] Example 3:

[0024] Crush 80 mesh iron holly raw material, take 5kg, add 75kg of water and heat to 60℃, keep for 4 hours, extract the extract, then add 75kg of water to 60℃ for 2 hours, combine the extract and concentrate to 120ml under reduced pressure, add the concentrated solution Azeotrope with 6L 99% methanol, then add 80g medicinal activated carbon for decolorization, adjust the pH of the decolorizing liquid with phosphoric acid, place the precipitate, filter impurities, adjust the filtrate with calcium hydroxide solution to adjust to neutral under reduced pressure and concentrate to alcohol-free, add 700ml water saturated n-butanol for extraction Three times, collect the n-butanol extraction layer, recover the n-butanol under reduced pressure, add a proper amount of water and place to crystallize to obtain 179g of crystals, add 3L of water to reflux for crystallization, filter out the crystals and reflux with 40% acetone solution to dissolve, filter and place Crysta...

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Abstract

The invention relates to a method for extracting syringin, comprising the following steps of: using Ilex rotunda as material, crushing the material to 20-80 meshes, adding 6-20 folds of water to extract for 2-3 times at 60-80 DEG C; concentrating the extraction liquid under reduced pressure, adding low-carbon alcohol to the extraction liquid for azeotropy, adding 0.5-2% of active carbon for decolorizing; adjusting the pH of decolorized liquid to 1-3, precipitating and filtering the impurity, adjusting the filtrate to be neutral by the aqueous alkali, concentrating the filtrate under reduced pressure until no alcohol exists, adding water to be saturated so as to extract n-butyl alcohol; collecting n-butyl alcohol extract liquor; recovering the n-butyl alcohol under reduced pressure, adding proper amount of water and storing the mixture to form crystal, filtering the crystal; dissolving the crystal with water and acetone solution for re-crystallization; and drying the crystal under reduced pressure to obtain the syringin product. By using the method for extracting the syringin, the one-time investment on devices for the method is less, process operation is simple and product content is high, so that the method is suitable for industrial production.

Description

Technical field: [0001] The invention belongs to the field of separation of natural products, in particular to a method for extracting syringin. Background technique: [0002] Syringin, also known as syringin, Zushimabingin, and glucoside A, is a phenylpropanoid compound, slightly soluble in cold water, slightly soluble in acetone, soluble in hot water, methanol, ethanol, almost insoluble in ether, Benzene, chloroform. Syringin has hemostatic and antitumor effects. [0003] Existing natural syringin is generally extracted from Acanthopanax senticosus, Iron holly, white clove and snow lotus, and there are many techniques. [0004] Such as the patent "high-purity syringin, preparation method and application", the method disclosed in this patent is to dissolve Acanthopanax acanthopanax extractum in hot water as a raw material, then let it stand, centrifuge, and the centrifugate is filtered and then subjected to macroporous resin chromatography. Column, first remove impuritie...

Claims

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Application Information

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IPC IPC(8): C07H15/203C07H1/08
Inventor 刘东锋杨成东
Owner NANJING ZELANG MEDICAL TECH
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