Method for extracting and refining rutin

A purification method and technology of organic solvent, applied in the field of extraction and purification of rutin, can solve the problems of difficulty in product purification, low product yield, low product content, etc., achieve low production cost, ensure extraction rate and yield, environmental protection low pollution effect

Active Publication Date: 2012-10-10
湖南莱崔尔生物科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] At present, the methods for producing rutin mainly include: 1, hot water extraction method, although this method is simple in process and low in equipment requirements, but the product yield is low and the quality is poor; 2, alkali extraction-acid precipitation method, this method prepares rutin Although the quality of the product is slightly better, the yield is low; 3. Solvent extraction method, although the yield of this method is guaranteed, the refining of the product is quite difficult, and the product content is low
It can be seen that the above methods have their own advantages and disadvantages.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] This embodiment includes the following steps:

[0023] (1) Extraction: take 50g of Sophora japonica, crush it to 50 mesh, extract with methanol three times, add 200mL of methanol for the first time, extract at 68°C, reflux for 3 hours, filter, and obtain the extract; add 150mL of methanol for the second time, Extract at 68°C, reflux for 2 hours, filter to obtain the extract; add methanol 150mL for the third time, extract at 68°C, reflux for 2 hours, filter to obtain the extract; combine the three extracts, concentrate into thick extract No methanol;

[0024] (2) Alkali dissolution-acid precipitation: first add 1000mL saturated lime water (containing 0.5wt% borax) to the thick extract, heat to 60°C, stir and dissolve for 2 hours, filter to obtain an alkaline filtrate, and then add alkaline Add 15wt% hydrochloric acid to the filtrate, adjust the pH value to 3, let it settle for 20 hours, filter, and dry the obtained filter residue at a temperature of 80°C for 12 hours to...

Embodiment 2

[0027] This embodiment includes the following steps:

[0028] (1) Extraction: take 50g of Sophora japonica, crush it to 50 mesh, extract three times with ethanol, add 200mL of ethanol for the first time, extract at 80°C, reflux for 3 hours, filter, and obtain the extract; add 150mL of ethanol for the second time, Extract at 80°C, reflux for 2 hours, filter to obtain the extract; add 150 mL of ethanol for the third time, extract at 80°C, extract at 80°C for 2 hours, filter to obtain the extract; combine the three extracts and concentrate into thick extract Ethanol-free;

[0029] (2) Alkali dissolution-acid precipitation: first add 1000 mL of saturated lime water (containing 0.5wt% borax) to the thick extract, heat to 60°C, stir and dissolve for 2 hours, filter to obtain an alkaline filtrate, and then add to the alkali Add 15wt% hydrochloric acid to the neutral filtrate, adjust the pH value to 3, let stand for precipitation for 20 hours, filter, and dry the resulting filter res...

Embodiment 3

[0032] This embodiment includes the following steps:

[0033] (1) Extraction: take 50g of buckwheat (dried), crush it to 50 mesh, extract three times with n-butanol, add 200mL of n-butanol for the first time, extract at 80°C, extract for 3 hours, and filter to obtain the extract; Add 150 mL of n-butanol for the second time, extract at 80°C, extract for 2 hours, and filter to obtain an extract; add 150 mL of n-butanol for the third time, extract at 80°C, extract for 2 hours, and filter to obtain an extract; combine Three extracts, concentrated until there is no n-butanol in the thick extract;

[0034] (2) Alkali dissolution-acid precipitation: first add 1000mL 2wt% potassium hydroxide aqueous solution (containing 0.5wt% borax) to the thick extract, heat to 65°C, stir and dissolve for 2 hours, filter to obtain an alkaline filtrate, Then add 12wt% sulfuric acid to the alkaline filtrate, adjust the pH value to 3.5, let it settle for 18 hours, filter, and dry the obtained filter r...

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PUM

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Abstract

A method for extracting and refining rutin comprises the following steps of (1) extraction: smashing raw materials, adding organic solvent into the smashed raw materials, performing extraction for 2-4 times, mixing extracting solution and concentrating the mixed extracting solution to thick extract with organic solvent content smaller than or equal to 5wt%; (2) alkali dissolution-acid sediment: adding alkaline water into the thick extract, then heating the mixture and stirring, filtering the heated mixture, regulating pH of alkaline filtrate to be 3-4, standing, filtering, drying to obtain a rutin pure product; and (3) mother liquor treatment: enabling obtained acid mother liquor to penetrate through a chromatographic column filled with resin, after the acid mother liquor penetrates through the chromatographic column, firstly using deionized water to wash a column bed until outflow liquid is neutral and colorless, introducing eluent into the chromatographic column and collecting eluate until outflow liquid is colorless, concentrating the eluate to the volume which is 5-10% of the original volume in a pressure reduction mode, cooling the concentrated eluate to achieve crystallization, filtering, using the deionized water to elute a filter cake, and drying the eluted filter cake to obtain a mother liquor rutin product. The prepared rutin is high in yield and purity, and the quality of the rutin reaches the international standard.

Description

technical field [0001] The invention relates to a method for extracting and refining rutin. Background technique [0002] Rutin (Rutin), which belongs to flavonoids, is also known as rutin, vitamin P, and purple quercetin; it not only reduces the permeability and fragility of capillaries, but also maintains and restores the normal elasticity of capillaries. It is used to prevent and treat hypertensive cerebral hemorrhage, diabetic retinal hemorrhage and hemorrhagic purpura. [0003] At present, the methods for producing rutin mainly include: 1, hot water extraction method, although this method is simple in process and low in equipment requirements, but the product yield is low and the quality is poor; 2, alkali extraction-acid precipitation method, this method prepares rutin Although the product quality is slightly better, the yield is on the low side; 3, solvent extraction method, although this method yield is guaranteed, the refining of the product is quite difficult, and...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07H17/07C07H1/08
Inventor 刘志强
Owner 湖南莱崔尔生物科技有限公司
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