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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 complicated process and high cost; extracting from Ilex holly adopts benzene degreasing, which is harmful to people and the environment Serious, the process is not suitable for industrialization

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] The raw material of iron holly is crushed to 20 mesh, take 1kg, add 15kg of water, heat to 80°C, keep warm for extraction for 3 hours, filter out the extract, add 8kg of water and keep at 80°C for 2 hours, filter out the extract, add 6kg of water and keep at 80°C For 2 hours, combine the three extracts and concentrate under reduced pressure to 100ml, add 1L of 95% ethanol to the concentrated solution to azeotrope, add 20g of medicinal activated carbon to decolorize, adjust the pH of the decolorized solution to 3 with hydrochloric acid, place the precipitate, filter impurities, and adjust the filtrate with sodium hydroxide solution Concentrate under reduced pressure until there is no alcohol, add 100ml of water to saturate n-butanol for extraction 4 times, collect the n-butanol extract layer, recover n-butanol under reduced pressure, add an appropriate amount of water and place it for crystallization to obtain 32g of crystals, add 300ml of water to reflux for crystallizati...

Embodiment 2

[0022] Grind the iron holly raw material into 60 meshes, take 1kg, add 20kg of water and heat to 70°C, keep it warm for extraction for 3 hours, filter the extract, add 10kg of water and keep it at 70°C for 2 hours, combine the extracts and concentrate them under reduced pressure to 150ml, add the concentrate to 1.5 L of 90% ethanol is azeotroped, plus 30 g of medicinal activated carbon for decolorization, the decolorization solution is adjusted to pH 1 with phosphoric acid, the precipitate is placed, and impurities are filtered, the filtrate is adjusted to neutrality with potassium hydroxide solution and concentrated under reduced pressure to no alcohol, and 150 ml of water-saturated n-butanol is added Extract 3 times, collect the n-butanol extraction layer, recover n-butanol under reduced pressure, add appropriate amount of water and place it for crystallization, and obtain 38 g of crystals, add 400 ml of water to reflux for crystallization, filter out the crystals and dissolve...

Embodiment 3

[0024] Grind the iron holly raw material into 80 meshes, take 5kg, add 75kg of water and heat to 60°C, keep warm for extraction for 4 hours, filter the extract, add 75kg of water and keep warm at 60°C for 2 hours, combine the extracts and concentrate them under reduced pressure to 120ml, add the concentrate to Azeotrope with 6L of 99% methanol, add 80g of medicinal activated carbon for decolorization, adjust the pH of the decolorization solution to pH2 with phosphoric acid, place the precipitate, filter impurities, adjust the filtrate to neutral with calcium hydroxide solution, concentrate under reduced pressure until alcohol-free, add 700ml of water saturated n-butanol for extraction 3 times, collect the n-butanol extraction layer, recover n-butanol under reduced pressure, add appropriate 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 then reflux with 40% acetone solution to dissolv...

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PUM

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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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