CN103923139B - A kind of method extracting rutin from the sophora bud - Google Patents
A kind of method extracting rutin from the sophora bud Download PDFInfo
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Abstract
The invention belongs to Extraction of rutin field, specifically a kind of method extracting rutin from the sophora bud.This preparation method utilizes the new sophora flower flower bud gathered to be starting raw material, degrading enzyme is eliminated through steam, after pulverizing and sieving, be main solvent with clarification liming, add the effective constituent rutin in oxidation inhibitor and the complexing of metal ion agent seepage pressure effects sophora bud, collect the percolate after filtering at times, and filter acid adjustment after adding Chinese medicine finings and polymeric adsorbent placement certain hour in proportion, the impure clear liquid in upper strata is discarded after rutin Precipitation, filter press, pH value is reconciled after product in the middle of filter press being added in the purified water of modulated good pH value again dissolution filter, filter press after placement crystallization, the rutin finished product meeting European Pharmacopoeia requirement is obtained after purified water washing drying.Rutin content >=95.0% of the present invention, product purity is high, and indices all reaches European Pharmacopoeia requirement, and leaching process does not adopt methyl alcohol, avoids methyl alcohol poisonous and be difficult to the problem removed.
Description
Technical field
The invention belongs to Extraction of rutin field, specifically a kind of method extracting rutin from the sophora bud.
Background technology
Rutin can be used as edible antioxidant and nutrient intensifier and accessory substance, there is the effect of vitamin P sample and anti-inflammatory action, the inflammation as tori seed oil causes animal eyes or skin can be reduced, there is antivirus action, and the effect of capillary permeability and fragility can be reduced, keep and recover the normal elasticity of capillary vessel.Rutin is present in the plants such as rue leaf, tobacco leaf, orange peel, tomato, Flos Sophorae Immaturus and Buckwheat Flower intensive amount especially abundant.The medicinal violaguercitrin of China raises from Flos Sophorae Immaturus.Utilize rutin to have acidity, in buck, solubleness is comparatively large, and with alkali salify and water-soluble, acid adding can make it become Acid precipitation, swim isolated principle.Filtrate, after washing, is adjusted to suitable pH value with after hot-water cure with clarification limewater extraction hydrochloric acid, leaves standstill crystallization, be separated, obtain violaguercitrin crude product, both obtained finished product through dissolving, recrystallize, drying by sophora bud flower.The sophora bud is the bud of leguminous plants Chinese scholartree.The sophora bud is produced in the ground such as Guangxi, Henan, Shandong, Shanxi, Shaanxi, Anhui, Hebei, Jiangsu, and existing implant mass base is with in Guangxi Region in recent years Quanzhou one.Guangxi and Vietnam's sophora bud quality good, yield is high, and because its special weather is beneficial to the growth of the sophora bud, it is low that it produces rutin impurity, and content is high.
At present, all rutin has been included in China's drug standard and European Pharmacopoeia, European Pharmacopoeia name is called: three hydration rutins, the rutin specification of quality that up-to-date European Pharmacopoeia requires is far above the national drug standards, its the key technical indexes is as follows: content 95.0 ~ 101.0%(is by dry product), moisture requirement is 7.5 ~ 9.5%, sulfated ash: be no more than 0.1%, insoluble methyl alcohol: be no more than 3%, light-absorbing impurity: the absorption value under 450nm and 800nm wavelength is no more than 0.10; To the limited requirement of impurity A, B, C and total impurities, detect related impurities by liquid phase chromatography.American Pharmacopeia NF11 version rutin standard-required in 1963 can only be met at present with the rutin that traditional technology is produced, reach European Pharmacopoeia requirement have to pass through dissolve with methanol refine, and refining inevitably the causing of the dissolving of methyl alcohol introduces methyl alcohol, but methyl alcohol has very large harm to HUMAN HEALTH, European Pharmacopoeia remains bound requirements to the methyl alcohol in product, is difficult to removing.Three hydration rutin molecular formula are as follows.
Summary of the invention
The object of the invention is to overcome existing Extraction of rutin preparation technology and there is the problems such as refining organic solution methyl alcohol is poisonous, the removal of methyl alcohol later stage is difficult, a kind of method extracting rutin from the sophora bud is provided.
The solution of the present invention is by realizing like this: a kind of method extracting rutin from the sophora bud, and gather sophora flower flower bud and carry out drying after hot steam cooker eliminates degrading enzyme, the sophora flower flower bud of drying carries out pulverizing and sieving obtaining bud flour, and the method step also comprises:
Step 1) seepage pressure effects: bud flour is put into percolate pot, and the clarification liming added in percolate pot containing oxidation inhibitor, complexing of metal ion agent extracts rutin, collects the percolate obtained.
Step 2) clarification removal of impurities: in step 1) add finings in the percolate that obtains, ratio=0.05 ~ the 0.1kg:1L of finings and percolate, after stirring, add macroporous adsorbent resin, ratio=0.1 ~ the 0.2L:2L of macroporous adsorbent resin and percolate, leave standstill 25 ~ 40min, cross and filter removing impurity by means of precipitation, obtain the extraction solution after removal of impurities.
Step 3) acid adjustment crystallization: toward step 2) obtain removal of impurities after extraction solution in add acid solution, regulate pH to 2.0 ~ 3.5, after rutin Precipitation, discard upper solution, containing precipitation solution carry out filter press, obtain rutin crude product.
Step 4) polishing purification: utilize pH value be 8.0 ~ 10.0 containing OH
-pure water solution dissolving step 3 again) the rutin crude product that obtains, after rutin crude product dissolves completely, recycling acid solution regulates containing rutin crude product solution pH to 2.0 ~ 3.5, leave standstill solution to separate out to rutin crystalline deposit, solution containing precipitation carries out filter press and obtains refined rutin product, with pH neutral purified water washing refined rutin product, having washed rear drying products to water content is 7.5 ~ 9.5%, obtains final rutin product.
As further restriction of the present invention, the antioxidant adopted in described seepage pressure effects is a kind of in S-WAT, sodium bisulfite, vitamins C (VC) or their mixture, and the content of antioxidant in clarification liming is 0.01 ~ 0.1%; Described complexing of metal ion agent is the mixture of any one or they in EDTA, monoethanolamine, diethanolamine, trolamine, ethylenediamine tetraacetic methene sodium phosphate (EDTMPS), diethylene triamine pentamethylene phosphonic salt (DETPMPS), and the content of complexing of metal ion agent in clarification liming is 0.01 ~ 0.1%; Described clarification liming is the Ca (OH) containing 0.05 ~ 0.15%
2.
As further restriction of the present invention, finings in described clarification removal step is natural traditional Chinese medicine finings KBT-ZTC, and natural traditional Chinese medicine finings KBT-ZTC is the natural traditional Chinese medicine finings that Ke Lier Bioisystech Co., Ltd produces, is made up of main solidifying agent A and auxiliary agent B; Described step 3) and 4) in the acid solution used be the hydrochloric acid HCl solution of 0.1 ~ 0.5mol/L or the sulfuric acid H of 0.1 ~ 0.5mol/L
2sO
4solution.
The present invention realize know-why be: this technique with the dry flower of the Chinese scholartree of Guangxi province for raw material, after pulverizing and sieving, be main solvent with clarification liming, add the effective constituent rutin in oxidation inhibitor and the complexing of metal ion agent seepage pressure effects sophora bud, collect the percolate after filtering at times, and filter acid adjustment after adding Chinese medicine finings and polymeric adsorbent placement certain hour in proportion, the impure clear liquid in upper strata is discarded after rutin Precipitation, filter press, pH value is reconciled after product in the middle of filter press being added in the purified water of modulated good pH value again dissolution filter, filter press after placement crystallization, the rutin finished product meeting European Pharmacopoeia requirement is obtained after purified water washing drying.
The present invention possesses following good result:
(1) in the rutin product for preparing of the present invention rutin content 95.0 ~ 101.0%(by dry product), moisture requirement is 7.5 ~ 9.5%, sulfated ash: be no more than 0.1%, insoluble methyl alcohol: be no more than 3%, light-absorbing impurity: the absorption value under 450nm and 800nm wavelength is no more than 0.10, indices reaches European Pharmacopoeia requirement.
(2) the present invention is by introducing Chinese medicine finings and polymeric adsorbent removal of impurities, can remove the impurity such as the plant chlorophyll in percolate, colloid, effectively improve product purity, alleviate follow-up removal of impurities pressure.
(3) the present invention changes traditional technology and first produces rutin crude product again by the technique of dissolve with methanol removing alcohol insoluble matter impurity, crosses to filter alcohol insoluble solids and the method for recrystallization in pure water that is used in improves product purity under the metasomite extracted adopts specific pH value and temperature with pure water after dissolving.No longer use organic solvent in process of production; to avoid in product organic solvent residual to the harm of HUMAN HEALTH; after present invention process improves; Product Process is tending towards simply, the production cycle shortens, product cost reduces 5 ~ 15%; saved the energy and manpower, product meets state guarantee, promotion, support, encourage growth environmental protection and energy saving policy requirements.
Accompanying drawing explanation
Fig. 1. a kind of schema extracting the method for rutin from the sophora bud of the present invention.
Embodiment
Describe a kind of method extracting rutin from the sophora bud of the present invention below in conjunction with embodiment and accompanying drawing, these descriptions are not be further limited content of the present invention.
Embodiment 1
Gather sophora flower flower bud 10kg to carry out drying after hot steam cooker eliminates degrading enzyme, the sophora flower flower bud of drying carries out pulverizing and sieving obtaining bud flour, and bud flour enters following steps and extracts:
Step 1) seepage pressure effects: bud flour is put into percolate pot, the clarification liming added in percolate pot containing oxidation inhibitor, complexing of metal ion agent extracts rutin, antioxidant is VC, the content of antioxidant VC in clarification liming is 0.1%, complexing of metal ion agent is EDTA, the content of complexing of metal ion agent in clarification liming is 0.1%, and clarification liming is the Ca (OH) containing 0.15%
2, collect the percolate obtained.
Step 2) clarification removal of impurities: in step 1) add natural traditional Chinese medicine finings KBT-ZTC in the percolate that obtains, ratio=the 0.1kg:1L of natural traditional Chinese medicine finings KBT-ZTC and percolate, after stirring, add macroporous adsorbent resin, ratio=the 0.2L:2L of macroporous adsorbent resin and percolate, leave standstill 40min, cross and filter removing impurity by means of precipitation, obtain the extraction solution after removal of impurities.
Step 3) acid adjustment crystallization: toward step 2) obtain removal of impurities after extraction solution in add acid solution, acid solution is the hydrochloric acid HCl solution of 0.3mol/L, regulates pH to 2.0, after rutin Precipitation, discards upper solution, solution containing precipitation carries out filter press, obtains rutin crude product.
Step 4) polishing purification: utilize pH value be 8.0 containing OH
-pure water solution dissolving step 3 again) the rutin crude product that obtains, after rutin crude product dissolves completely, recycling acid solution regulates containing rutin crude product solution pH to 3.5, acid solution is the hydrochloric acid HCl solution of 0.3mol/L, leave standstill solution to separate out to rutin crystalline deposit, the solution containing precipitation carries out filter press and obtains refined rutin product, with pH neutral purified water washing refined rutin product, having washed rear drying products to water content is 9.0%, obtains final rutin product.
Embodiment 2
Gather sophora flower flower bud 10kg to carry out drying after hot steam cooker eliminates degrading enzyme, the sophora flower flower bud of drying carries out pulverizing and sieving obtaining bud flour, and bud flour enters following steps and extracts:
Step 1) seepage pressure effects: bud flour is put into percolate pot, the clarification liming added in percolate pot containing oxidation inhibitor, complexing of metal ion agent extracts rutin, antioxidant is sodium bisulfite, the content of sodium bisulfite antioxidant in clarification liming is 0.05%, complexing of metal ion agent is monoethanolamine, diethanolamine, trolamine mix according to weight 1:1:1, the content of complexing of metal ion agent in clarification liming is 0.01%, and clarification liming is the Ca (OH) containing 0.05%
2, collect the percolate obtained.
Step 2) clarification removal of impurities: in step 1) add natural traditional Chinese medicine finings KBT-ZTC in the percolate that obtains, ratio=the 0.06kg:1L of natural traditional Chinese medicine finings KBT-ZTC and percolate, after stirring, add macroporous adsorbent resin, ratio=the 0.1L:2L of macroporous adsorbent resin and percolate, leave standstill 30min, cross and filter removing impurity by means of precipitation, obtain the extraction solution after removal of impurities.
Step 3) acid adjustment crystallization: toward step 2) obtain removal of impurities after extraction solution in add acid solution, acid solution is the hydrochloric acid HCl solution of 0.2mol/L, regulates pH to 2.0, after rutin Precipitation, discards upper solution, solution containing precipitation carries out filter press, obtains rutin crude product.
Step 4) polishing purification: utilize pH value be 8.0 containing OH
-pure water solution dissolving step 3 again) the rutin crude product that obtains, after rutin crude product dissolves completely, recycling acid solution regulates containing rutin crude product solution pH to 2.5, acid solution is the hydrochloric acid HCl solution of 0.2mol/L, leave standstill solution to separate out to rutin crystalline deposit, the solution containing precipitation carries out filter press and obtains refined rutin product, with pH neutral purified water washing refined rutin product, having washed rear drying products to water content is 9.5%, obtains final rutin product.
Embodiment 3
Gather sophora flower flower bud 10kg to carry out drying after hot steam cooker eliminates degrading enzyme, the sophora flower flower bud of drying carries out pulverizing and sieving obtaining bud flour, and bud flour enters following steps and extracts:
Step 1) seepage pressure effects: bud flour is put into percolate pot, the clarification liming added in percolate pot containing oxidation inhibitor, complexing of metal ion agent extracts rutin, antioxidant is S-WAT, the content of S-WAT antioxidant in clarification liming is 0.05%, complexing of metal ion agent is diethylene triamine pentamethylene phosphonic salt (DETPMPS), the content of complexing of metal ion agent in clarification liming is 0.1%, and clarification liming is the Ca (OH) containing 0.05%
2, collect the percolate obtained.
Step 2) clarification removal of impurities: in step 1) add natural traditional Chinese medicine finings KBT-ZTC in the percolate that obtains, ratio=0.05 ~ the 0.kg:1L of natural traditional Chinese medicine finings KBT-ZTC and percolate, after stirring, add macroporous adsorbent resin, ratio=0.1 ~ the 0.L:2L of macroporous adsorbent resin and percolate, leave standstill 25min, cross and filter removing impurity by means of precipitation, obtain the extraction solution after removal of impurities.
Step 3) acid adjustment crystallization: toward step 2) obtain removal of impurities after extraction solution in add acid solution, acid solution is the sulfuric acid H of 0.1mol/L
2sO
4solution, regulates pH to 3.5, after rutin Precipitation, discards upper solution, and the solution containing precipitation carries out filter press, obtains rutin crude product.
Step 4) polishing purification: utilize pH value be 9.0 containing OH
-pure water solution dissolving step 3 again) the rutin crude product that obtains, after rutin crude product dissolves completely, recycling acid solution regulates containing rutin crude product solution pH to 2.0, and acid solution is the sulfuric acid H of 0.1mol/L
2sO
4solution, leave standstill solution and separate out to rutin crystalline deposit, the solution containing precipitation carries out filter press and obtains refined rutin product, and with pH neutral purified water washing refined rutin product, having washed rear drying products to water content is 7.5%, obtains final rutin product.
Embodiment 4
Gather sophora flower flower bud 10kg to carry out drying after hot steam cooker eliminates degrading enzyme, the sophora flower flower bud of drying carries out pulverizing and sieving obtaining bud flour, and bud flour enters following steps and extracts:
Step 1) seepage pressure effects: bud flour is put into percolate pot, the clarification liming added in percolate pot containing oxidation inhibitor, complexing of metal ion agent extracts rutin, antioxidant is S-WAT, VC is that 1:1 is mixed to get according to weight ratio, the content of antioxidant in clarification liming is 0.1%, complexing of metal ion agent is ethylenediamine tetraacetic methene sodium phosphate (EDTMPS), the content of complexing of metal ion agent in clarification liming is 0.05%, and clarification liming is the Ca (OH) containing 0.15%
2, collect the percolate obtained.
Step 2) clarification removal of impurities: in step 1) add natural traditional Chinese medicine finings KBT-ZTC in the percolate that obtains, ratio=the 0.08kg:1L of natural traditional Chinese medicine finings KBT-ZTC and percolate, after stirring, add macroporous adsorbent resin, ratio=the 0.15L:2L of macroporous adsorbent resin and percolate, leave standstill 35min, cross and filter removing impurity by means of precipitation, obtain the extraction solution after removal of impurities.
Step 3) acid adjustment crystallization: toward step 2) obtain removal of impurities after extraction solution in add acid solution, acid solution is the hydrochloric acid HCl solution of 0.5mol/L, regulates pH to 2.0, after rutin Precipitation, discards upper solution, solution containing precipitation carries out filter press, obtains rutin crude product.
Step 4) polishing purification: utilize pH value be 10.0 containing OH
-pure water solution dissolving step 3 again) the rutin crude product that obtains, after rutin crude product dissolves completely, recycling acid solution regulates containing rutin crude product solution pH to 2.0, acid solution is the hydrochloric acid HCl solution of 0.5mol/L, leave standstill solution to separate out to rutin crystalline deposit, the solution containing precipitation carries out filter press and obtains refined rutin product, with pH neutral purified water washing refined rutin product, having washed rear drying products to water content is 8.5%, obtains final rutin product.
Embodiment 5
Gather sophora flower flower bud 10kg to carry out drying after hot steam cooker eliminates degrading enzyme, the sophora flower flower bud of drying carries out pulverizing and sieving obtaining bud flour, and bud flour enters following steps and extracts:
Step 1) seepage pressure effects: bud flour is put into percolate pot, the clarification liming added in percolate pot containing oxidation inhibitor, complexing of metal ion agent extracts rutin, antioxidant is S-WAT, sodium bisulfite is mixed to get according to weight ratio 1:1, the content of antioxidant in clarification liming is 0.05%, complexing of metal ion agent is EDTA, monoethanolamine is mixed to get according to weight ratio 1:1, the content of complexing of metal ion agent in clarification liming is 0.1%, and clarification liming is the Ca (OH) containing 0.1%
2, collect the percolate obtained.
Step 2) clarification removal of impurities: in step 1) add natural traditional Chinese medicine finings KBT-ZTC in the percolate that obtains, ratio=the 0.1kg:1L of natural traditional Chinese medicine finings KBT-ZTC and percolate, after stirring, add macroporous adsorbent resin, ratio=the 0.2L:2L of macroporous adsorbent resin and percolate, leave standstill 40min, cross and filter removing impurity by means of precipitation, obtain the extraction solution after removal of impurities.
Step 3) acid adjustment crystallization: toward step 2) obtain removal of impurities after extraction solution in add acid solution, acid solution is the sulfuric acid H of 0.2mol/L
2sO
4solution, regulates pH to 3.0, after rutin Precipitation, discards upper solution, and the solution containing precipitation carries out filter press, obtains rutin crude product.
Step 4) polishing purification: utilize pH value be 8.0 containing OH
-pure water solution dissolving step 3 again) the rutin crude product that obtains, after rutin crude product dissolves completely, recycling acid solution regulates containing rutin crude product solution pH to 3.0, and acid solution is the sulfuric acid H of 0.2mol/L
2sO
4solution, leave standstill solution and separate out to rutin crystalline deposit, the solution containing precipitation carries out filter press and obtains refined rutin product, and with pH neutral purified water washing refined rutin product, having washed rear drying products to water content is 7.5 ~ 9.5%, obtains final rutin product.
In the rutin product that embodiment 1 ~ 5 prepares, rutin content 95.0 ~ 101.0%(is by dry product), moisture requirement is 7.5 ~ 9.5%, sulfated ash: be no more than 0.1%, insoluble methyl alcohol: be no more than 3%, light-absorbing impurity: the absorption value under 450nm and 800nm wavelength is no more than 0.10, indices reaches European Pharmacopoeia requirement.
The above embodiment of the present invention scheme is only can not limit the present invention to explanation of the present invention, the scope of product moiety of the present invention, component proportions, preparation method's parameter is indicated in claim, and the scope of parameter of the present invention is not pointed out in above-mentioned explanation, therefore, any change in the implication suitable with claims of the present invention and scope, is all considered to be and is included in the scope of claims.The present invention is through researchist's long term operation experience accumulation of the extraction preparation method of multidigit rutin, and is created by creative work.
Claims (3)
1. from the sophora bud, extract a method for rutin, gather sophora flower flower bud and carry out drying after hot steam cooker eliminates degrading enzyme, the sophora flower flower bud of drying carries out pulverizing and sieving obtaining bud flour, and it is characterized in that, the method step also comprises:
Step 1) seepage pressure effects: bud flour is put into percolate pot, and the clarification liming added in percolate pot containing oxidation inhibitor, complexing of metal ion agent extracts rutin, collects the percolate obtained;
Step 2) clarification removal of impurities: in step 1) add finings in the percolate that obtains, ratio=0.05 ~ the 0.1kg:1L of finings and percolate, after stirring, add macroporous adsorbent resin, ratio=0.1 ~ the 0.2L:2L of macroporous adsorbent resin and percolate, leave standstill 25 ~ 40min, cross and filter removing impurity by means of precipitation, obtain the extraction solution after removal of impurities;
Step 3) acid adjustment crystallization: toward step 2) obtain removal of impurities after extraction solution in add acid solution, regulate pH to 2.0 ~ 3.5, after rutin Precipitation, discard upper solution, containing precipitation solution carry out filter press, obtain rutin crude product;
Step 4) polishing purification: utilize pH value be 8.0 ~ 10.0 containing OH
-pure water solution dissolving step 3 again) the rutin crude product that obtains, after rutin crude product dissolves completely, recycling acid solution regulates containing rutin crude product solution pH to 2.0 ~ 3.5, leave standstill solution to separate out to rutin crystalline deposit, solution containing precipitation carries out filter press and obtains refined rutin product, with pH neutral purified water washing refined rutin product, wash rear drying products to water content < 10%, obtained final rutin product;
Finings in described clarification removal step is natural traditional Chinese medicine finings KBT-ZTC; Described step 3) and 4) in the acid solution used be the hydrochloric acid HCl solution of 0.1 ~ 0.5mol/L or the sulfuric acid H of 0.1 ~ 0.5mol/L
2sO
4solution.
2. a kind of method extracting rutin from the sophora bud according to claim 1, it is characterized in that, the antioxidant adopted in described seepage pressure effects is one in S-WAT, sodium bisulfite, vitamins C or their mixture, and the content of antioxidant in clarification liming is 0.01 ~ 0.1%.
3. a kind of method extracting rutin from the sophora bud according to any one of right 1 or 2, it is characterized in that, the mixture of any one or they in described complexing of metal ion agent ethylenediamine tetraacetic acid (EDTA), monoethanolamine, diethanolamine, trolamine, ethylenediamine tetraacetic methene sodium phosphate, diethylene triamine pentamethylene phosphonic salt, the content of complexing of metal ion agent in clarification liming is 0.01 ~ 0.1%; Described clarification liming is the Ca(OH containing 0.05 ~ 0.15%)
2 .
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105647230B (en) * | 2016-03-10 | 2018-01-02 | 常州大学 | A kind of extracting method of sophora bud natural dye and application |
| CN106046080A (en) * | 2016-05-30 | 2016-10-26 | 铜陵东晟生态农业科技有限公司 | Method for purifying rutin |
| CN107827942A (en) * | 2017-11-25 | 2018-03-23 | 衡阳县华盛达农林科技有限公司 | The method of purification of rutin |
| CN108047292A (en) * | 2018-01-26 | 2018-05-18 | 湘潭大学 | A kind of method that high-purity rutoside is extracted from the sophora bud |
| CN109111493B (en) * | 2018-10-12 | 2021-08-10 | 河南精康制药有限公司 | Raw material refining method for preparing troxerutin for injection |
| CN111635443A (en) * | 2020-06-15 | 2020-09-08 | 深圳市蜜踪生物科技有限公司 | Sophora flower extraction process |
| CN113416224A (en) * | 2021-06-18 | 2021-09-21 | 山东东宇生态科技有限公司 | Preparation system and method for extracting rutin from sophora flower buds |
| CN114480139A (en) * | 2022-01-24 | 2022-05-13 | 黄淮学院 | Screening method of rutin degrading enzyme high-yield bacteria |
| CN116870048A (en) * | 2023-06-27 | 2023-10-13 | 成都市柏林生物科技开发有限公司 | Sophora flower extract and preparation method thereof |
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