CN104098635B - Method for extracting rutin from sophora flower bud - Google Patents
Method for extracting rutin from sophora flower bud Download PDFInfo
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- CN104098635B CN104098635B CN201410390859.8A CN201410390859A CN104098635B CN 104098635 B CN104098635 B CN 104098635B CN 201410390859 A CN201410390859 A CN 201410390859A CN 104098635 B CN104098635 B CN 104098635B
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- flos sophorae
- sophorae immaturus
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- JMGZEFIQIZZSBH-UHFFFAOYSA-N Bioquercetin Natural products CC1OC(OCC(O)C2OC(OC3=C(Oc4cc(O)cc(O)c4C3=O)c5ccc(O)c(O)c5)C(O)C2O)C(O)C(O)C1O JMGZEFIQIZZSBH-UHFFFAOYSA-N 0.000 title claims abstract description 54
- IVTMALDHFAHOGL-UHFFFAOYSA-N eriodictyol 7-O-rutinoside Natural products OC1C(O)C(O)C(C)OC1OCC1C(O)C(O)C(O)C(OC=2C=C3C(C(C(O)=C(O3)C=3C=C(O)C(O)=CC=3)=O)=C(O)C=2)O1 IVTMALDHFAHOGL-UHFFFAOYSA-N 0.000 title claims abstract description 54
- FDRQPMVGJOQVTL-UHFFFAOYSA-N quercetin rutinoside Natural products OC1C(O)C(O)C(CO)OC1OCC1C(O)C(O)C(O)C(OC=2C(C3=C(O)C=C(O)C=C3OC=2C=2C=C(O)C(O)=CC=2)=O)O1 FDRQPMVGJOQVTL-UHFFFAOYSA-N 0.000 title claims abstract description 54
- IKGXIBQEEMLURG-BKUODXTLSA-N rutin Chemical compound O[C@H]1[C@H](O)[C@@H](O)[C@H](C)O[C@@H]1OC[C@H]1[C@H](O)[C@@H](O)[C@H](O)[C@@H](OC=2C(C3=C(O)C=C(O)C=C3OC=2C=2C=C(O)C(O)=CC=2)=O)O1 IKGXIBQEEMLURG-BKUODXTLSA-N 0.000 title claims abstract description 54
- ALABRVAAKCSLSC-UHFFFAOYSA-N rutin Natural products CC1OC(OCC2OC(O)C(O)C(O)C2O)C(O)C(O)C1OC3=C(Oc4cc(O)cc(O)c4C3=O)c5ccc(O)c(O)c5 ALABRVAAKCSLSC-UHFFFAOYSA-N 0.000 title claims abstract description 54
- 235000005493 rutin Nutrition 0.000 title claims abstract description 54
- 229960004555 rutoside Drugs 0.000 title claims abstract description 54
- 238000000034 method Methods 0.000 title claims abstract description 25
- 241000219784 Sophora Species 0.000 title abstract 3
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 claims abstract description 26
- 238000000605 extraction Methods 0.000 claims abstract description 18
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 17
- 102000004190 Enzymes Human genes 0.000 claims abstract description 13
- 108090000790 Enzymes Proteins 0.000 claims abstract description 13
- 238000001035 drying Methods 0.000 claims abstract description 11
- 238000001914 filtration Methods 0.000 claims abstract description 11
- 229920001213 Polysorbate 20 Polymers 0.000 claims abstract description 8
- 239000000256 polyoxyethylene sorbitan monolaurate Substances 0.000 claims abstract description 8
- 235000010486 polyoxyethylene sorbitan monolaurate Nutrition 0.000 claims abstract description 8
- 239000000706 filtrate Substances 0.000 claims description 31
- 241000628997 Flos Species 0.000 claims description 23
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 20
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 15
- 230000008569 process Effects 0.000 claims description 10
- 239000012043 crude product Substances 0.000 claims description 9
- 239000000284 extract Substances 0.000 claims description 8
- 229910021538 borax Inorganic materials 0.000 claims description 7
- 239000008367 deionised water Substances 0.000 claims description 7
- 229910021641 deionized water Inorganic materials 0.000 claims description 7
- 239000004328 sodium tetraborate Substances 0.000 claims description 7
- 235000010339 sodium tetraborate Nutrition 0.000 claims description 7
- 238000002137 ultrasound extraction Methods 0.000 claims description 6
- 239000002253 acid Substances 0.000 claims description 5
- 229910052799 carbon Inorganic materials 0.000 claims description 5
- 239000013078 crystal Substances 0.000 claims description 5
- 239000008187 granular material Substances 0.000 claims description 5
- 238000010438 heat treatment Methods 0.000 claims description 5
- 230000020477 pH reduction Effects 0.000 claims description 5
- 238000003756 stirring Methods 0.000 claims description 5
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 4
- UIIMBOGNXHQVGW-DEQYMQKBSA-M Sodium bicarbonate-14C Chemical compound [Na+].O[14C]([O-])=O UIIMBOGNXHQVGW-DEQYMQKBSA-M 0.000 claims description 4
- 239000002994 raw material Substances 0.000 claims description 4
- 238000009210 therapy by ultrasound Methods 0.000 claims description 2
- 239000004094 surface-active agent Substances 0.000 abstract description 5
- 238000005406 washing Methods 0.000 abstract description 4
- 238000002425 crystallisation Methods 0.000 abstract description 3
- 230000008025 crystallization Effects 0.000 abstract description 3
- 238000004519 manufacturing process Methods 0.000 abstract description 2
- 230000009849 deactivation Effects 0.000 abstract 1
- 239000007788 liquid Substances 0.000 abstract 1
- 238000007670 refining Methods 0.000 abstract 1
- 239000000126 substance Substances 0.000 description 4
- 230000000694 effects Effects 0.000 description 3
- 230000003647 oxidation Effects 0.000 description 3
- 238000007254 oxidation reaction Methods 0.000 description 3
- 230000003213 activating effect Effects 0.000 description 2
- 238000007664 blowing Methods 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 239000003814 drug Substances 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 230000007062 hydrolysis Effects 0.000 description 2
- 238000006460 hydrolysis reaction Methods 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 241000196324 Embryophyta Species 0.000 description 1
- 208000032843 Hemorrhage Diseases 0.000 description 1
- 208000031226 Hyperlipidaemia Diseases 0.000 description 1
- 206010020772 Hypertension Diseases 0.000 description 1
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 1
- 208000004880 Polyuria Diseases 0.000 description 1
- 235000010586 Sophora japonica Nutrition 0.000 description 1
- 244000046101 Sophora japonica Species 0.000 description 1
- 229930013930 alkaloid Natural products 0.000 description 1
- 150000003797 alkaloid derivatives Chemical class 0.000 description 1
- 230000000954 anitussive effect Effects 0.000 description 1
- 230000003266 anti-allergic effect Effects 0.000 description 1
- 230000003110 anti-inflammatory effect Effects 0.000 description 1
- 239000003963 antioxidant agent Substances 0.000 description 1
- 230000003078 antioxidant effect Effects 0.000 description 1
- 235000006708 antioxidants Nutrition 0.000 description 1
- 229940124584 antitussives Drugs 0.000 description 1
- 239000011260 aqueous acid Substances 0.000 description 1
- 210000004369 blood Anatomy 0.000 description 1
- 239000008280 blood Substances 0.000 description 1
- AXCZMVOFGPJBDE-UHFFFAOYSA-L calcium dihydroxide Chemical compound [OH-].[OH-].[Ca+2] AXCZMVOFGPJBDE-UHFFFAOYSA-L 0.000 description 1
- BVKZGUZCCUSVTD-UHFFFAOYSA-N carbonic acid Chemical compound OC(O)=O BVKZGUZCCUSVTD-UHFFFAOYSA-N 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000007795 chemical reaction product Substances 0.000 description 1
- 229940126678 chinese medicines Drugs 0.000 description 1
- 239000000084 colloidal system Substances 0.000 description 1
- 239000000470 constituent Substances 0.000 description 1
- 239000002537 cosmetic Substances 0.000 description 1
- 206010012601 diabetes mellitus Diseases 0.000 description 1
- 235000014113 dietary fatty acids Nutrition 0.000 description 1
- PCHPORCSPXIHLZ-UHFFFAOYSA-N diphenhydramine hydrochloride Chemical compound [Cl-].C=1C=CC=CC=1C(OCC[NH+](C)C)C1=CC=CC=C1 PCHPORCSPXIHLZ-UHFFFAOYSA-N 0.000 description 1
- 230000035619 diuresis Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 230000003203 everyday effect Effects 0.000 description 1
- 239000000194 fatty acid Substances 0.000 description 1
- 229930195729 fatty acid Natural products 0.000 description 1
- 150000004665 fatty acids Chemical class 0.000 description 1
- 229930003935 flavonoid Natural products 0.000 description 1
- 229930182486 flavonoid glycoside Natural products 0.000 description 1
- -1 flavonoid glycoside compound Chemical class 0.000 description 1
- 150000002215 flavonoids Chemical class 0.000 description 1
- 235000017173 flavonoids Nutrition 0.000 description 1
- 235000013305 food Nutrition 0.000 description 1
- 229930182470 glycoside Natural products 0.000 description 1
- 150000002338 glycosides Chemical class 0.000 description 1
- 235000013402 health food Nutrition 0.000 description 1
- 210000003677 hemocyte Anatomy 0.000 description 1
- 229940000351 hemocyte Drugs 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 125000004435 hydrogen atom Chemical class [H]* 0.000 description 1
- 206010020718 hyperplasia Diseases 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 230000000415 inactivating effect Effects 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 230000002265 prevention Effects 0.000 description 1
- 238000010298 pulverizing process Methods 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 150000003839 salts Chemical group 0.000 description 1
- 238000004904 shortening Methods 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 238000002604 ultrasonography Methods 0.000 description 1
- 230000008728 vascular permeability Effects 0.000 description 1
- 239000000341 volatile oil Substances 0.000 description 1
- 239000001052 yellow pigment Substances 0.000 description 1
Classifications
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/50—Improvements relating to the production of bulk chemicals
- Y02P20/54—Improvements relating to the production of bulk chemicals using solvents, e.g. supercritical solvents or ionic liquids
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- Saccharide Compounds (AREA)
- Pharmaceuticals Containing Other Organic And Inorganic Compounds (AREA)
Abstract
The invention discloses a method for extracting rutin from sophora flower bud. The method includes the following steps: breaking dry sophora flower bud, adopting supercritical CO2 to conduct enzyme deactivation, conducting washing and drying, then adding a surfactant Tween20 and OP-15 with reasonable ratio and the like, conducting ultrasonic auxiliary extraction through 60%-70% ethanol, conducting standing crystallization on the extracting liquid, conducting extracting filtering to obtain a rutin coarse product, conducting n-butyl alcohol refining on the rutin coarse product, conducting standing crystallization on the rutin coarse product, drying the rutin coarse product under the temperature of 130 DEG C to obtain a rutin finished product with the purity higher than 98% and the yield higher than 23%. The method is simple in operation, high in extraction efficiency and applicable to actual production.
Description
Technical field
The application is related to a kind of method extracting rutin from the Flos Sophorae Immaturus.
Background technology
The Flos Sophorae Immaturus are dried flower and alabastrum for leguminous plant Sophora japonica L., the history being used as medicine existing more than 2000 year, Shennong's Herbal
It is classified as top grade.The rutin containing in the Flos Sophorae Immaturus, also known as rutin, rutin, belongs to flavonoid glycoside compound, can reduce hair
Thin vascular permeability and fragility, promote hyperplasia and prevent hemocyte cohesion, also have antiinflammatory, antiallergic, diuresis, antitussive,
Waiting of blood fat reducing acts on.Rutin clinically have been used as hypertension auxiliary treatment, prevent because rutin lack lead to other
Hemorrhage, and prevention and treatment diabetes and merging hyperlipidemia.In addition, rutin is as natural antioxidant with using yellow
Pigment, is also widely used in health food and cosmetic kind.Rutin in Flos Sophorae Immaturus dry in the sun, washing, pulverizing, extraction process, easily
It is subject to coexist in the Folium Symplocoris Caudatae enzyme effect in the Flos Sophorae Immaturus and hydrolyze, therefore, enzyme denaturing or reduce enzyme before extracting or in extraction process
Activity is particularly significant.In prior art adopt enzyme inactivating method mainly have dry blowing, ultraviolet irradiate,60Co irradiates, microwave deactivating enzyme
Deng, wherein dry blowing temperature height, can cause hydrolysis and the oxidation of rutin while enzyme denaturing, part rutin also can be led to be dissolved in heat
Water and run off；Though and ultraviolet irradiate can effective enzyme denaturing, the used time is longer, and cost is also high, makes production efficiency reduction.With surface
Activating agent produces and the widely using of the field such as water process in chemical industry, food, article of everyday use, water insoluble or be difficult in a lot of Chinese medicines
It is dissolved in the effective ingredient of water, such as Flavonoid substances, alkaloid, volatile oil etc., can be by surfactant on its surface or boundary
Form adsorption on face, or form molecular aggregate in the solution, and then change these compositions dissolubility in aqueous,
Improve the extraction efficiency of Chinese medicine, reduce extraction cost, the feature of safety and environmental protection.
There is the report assisting Extraction of rutin using surfactant in prior art, but adopt a kind of surfactant more.
As Li Jinxiu etc. (" linguistic term of Rutin Extracting Technology ", Li Jinxiu, Gong Shengzhao, Huang Qiujin, Guangdong chemical industry, 2003 the 1st
Phase, p15) employ the extraction that following methods carry out rutin: the Flos Sophorae Immaturus are pulverized, and add the water of 5 times amount, adjust ph8 with lime water
～9, it is 50～60 DEG C of extraction 20～30min in temperature, filter, repeatedly extract 3 times by similarity condition, filtrate adjusts ph with hydrochloric acid
For 3, addition 0.5% surfactant op, it is incubated 10min at 60～70 DEG C, stands 30min, filter, washing, dry, obtain rue
Fragrant glycoside product yield 18.4%, content 96%.
Content of the invention
The application aims to provide a kind of new method extracting rutin from the Flos Sophorae Immaturus.
The method of the invention comprises the following steps:
(1) clean enzyme denaturing: be crushed to 20～80 mesh by the Flos Sophorae Immaturus are dried, add temperature to be 30～40 DEG C, the acid of ph=4～5
After water, insert supercritical co2In extraction equipment, pressure be 30mpa, temperature be 30～40 DEG C at process 20～40min, afterwards
It is 0～5 DEG C using temperature, the acid rinsing of ph=4～5 dries twice afterwards；
(2) extract: the Flos Sophorae Immaturus granule after drying adds 1～5% Borax, 1～5% na2so3With the 60 of 15-30 times～
In 70% ethanol, adjust ph to 9～10 using sodium bicarbonate, add 0.3～0.4% tween 20 and 0.05～0.2%
Op-15, under conditions of 20～30khz, 30～50 DEG C, lucifuge ultrasonic extraction 10～30min, filters afterwards, filtrate 30～
At 50 DEG C, lucifuge is standby；Filtering residue is extracted once with above-mentioned same condition again, and the filtrate obtaining is merged with filtrate before, Xiang He
And after filtrate in add 5% activated carbon, lucifuge stirring 10min at 30～50 DEG C, the acidification of filtrate after carbon removal will be filtered to ph=3
～4, stand 20～30min, sucking filtration obtains rutin crude product；
(3) refine: rutin crude product is placed in baking oven, dries to no alcohol taste at 40 DEG C, then be gradually heating to 130 DEG C of bakings
Dry, the rutin that is dried obtaining is added and is heated in n-butyl alcohol dissolving, filters, add deionized water in filtrate, using 20～
The ultrasonic lucifuge process 20～30min at 0～5 DEG C of 30khz, stands still for crystals and dries at 130 DEG C, obtain purity 98% and reach
Above rutin, yield reaches more than 23%.
Further, in step (1) of the present invention, the time preferred 40min of destroy the enzyme treatment；Described sour water can be salt
Aqueous acid.
Further, in step (2) of the present invention, it is preferably added to 3～4% Borax and 1% na2so3.
Further, in step (2) of the present invention, be preferably added to 0.35～0.45% tween 20 and 0.05～
0.15% op-15.
Further, in step (2) of the present invention, the condition of ultrasonic extraction preferably carries at 30khz, 40～50 DEG C
Take 15～25min；
Further, in step (3) of the present invention, the ratio that adds the volume of n-butyl alcohol and Flos Sophorae Immaturus raw materials quality is 20～
30ml/g；The volume of deionized water is added to be 2～3ml/g with the ratio of Flos Sophorae Immaturus raw materials quality；The condition of ultrasonic Treatment preferably exists
20～30min is processed under 30 khz.
The present invention adopts supercritical co2Carry out enzyme denaturing, the used time is short, and rutin is in supercritical co2Under the conditions of not readily dissolve, no
Hydrolysis, oxidation and the loss of rutin can be led to, remain the active constituent content of rutin to greatest extent；The surface of rational proportion
Activating agent tween 20 and op-15 makes extraction time and crystallization time all have shortening, and extraction efficiency improves, then is aided with ultrasound wave,
Oxidation wastage in extraction process for the rutin is made to reduce, yield increases substantially.Using n-butyl alcohol, rutin is refined, Ke Yiyou
Effect removes the impurity such as residual colloid, fatty acid, improves the purity of rutin.From the point of view of comprehensive each step of the present invention, this
Bright methods described is easy and simple to handle, extraction efficiency high it is adaptable to produce reality.
Brief description
Fig. 1 is rutin standard substance hplc spectrogram.
Fig. 2 is the hplc spectrogram of rutin end-product in embodiment 2.
Specific embodiment
Embodiment 1
50g is dried the Flos Sophorae Immaturus and is crushed to 40 mesh, add temperature to be 40 DEG C, after the sour water of ph=4～5, insert supercritical co2
In extraction equipment, process 20～40min at pressure 30mpa, 40 DEG C of temperature, be 0～5 DEG C using temperature afterwards, ph=4～5
Acid rinsing dry afterwards twice；Flos Sophorae Immaturus granule after drying adds 3% Borax, 1% na2so3In 25 times of 60% ethanol,
Adjust ph to 9～10 using sodium bicarbonate, add 0.35% tween 20 and 0.15% op-15,30khz, 40 DEG C
Under the conditions of lucifuge ultrasonic extraction 20min, filter afterwards, filtrate lucifuge at 40 DEG C is standby；Filtering residue is again with above-mentioned same
Condition is extracted once, and the filtrate obtaining is merged with filtrate before, adds 5% activated carbon, lucifuge at 40 DEG C in the filtrate to after merge
Stirring 10min, will filter the acidification of filtrate after carbon removal to ph=3～4, stands 20min, sucking filtration obtains rutin crude product；By rutin crude product
It is placed in baking oven, dries to no alcohol taste at 40 DEG C, then be gradually heating to 130 DEG C of drying, the rutin that is dried obtaining is added
Be heated in 1300ml n-butyl alcohol dissolve, filter, in filtrate add 130ml deionized water, using 30khz ultrasonic 0～5
At DEG C, lucifuge processes 20min, stands still for crystals, and dries, obtain the rutin 11.61g of purity 98.33%, yield 23.21% at 130 DEG C.
Embodiment 2
80g is dried the Flos Sophorae Immaturus and is crushed to 50 mesh, add temperature to be 40 DEG C, after the sour water of ph=4～5, insert supercritical co2
In extraction equipment, process 30min at pressure 30mpa, 40 DEG C of temperature, be 4 DEG C using temperature afterwards, the acid-water washing of ph=4～5
Wash and dry afterwards twice；Flos Sophorae Immaturus granule after drying adds 4% Borax, 1% na2so3In 20 times of 70% ethanol, using carbonic acid
Hydrogen sodium adjusts ph to 9～10, adds 0.4% tween 20 and 0.1% op-15, lucifuge under conditions of 30khz, 40 DEG C
Ultrasonic extraction 25min, filters afterwards, and filtrate lucifuge at 40 DEG C is standby；Filtering residue extracts one with above-mentioned same condition again
Secondary, the filtrate obtaining is merged with filtrate before, adds 5% activated carbon in the filtrate to after merge, lucifuge stirring 10min at 40 DEG C,
The acidification of filtrate after carbon removal will be filtered to ph=3～4, stand 25min, sucking filtration obtains rutin crude product；Rutin crude product is placed in baking oven
In, dry to no alcohol taste at 40 DEG C, then be gradually heating to 130 DEG C drying, by obtain be dried rutin add 2l n-butyl alcohol in plus
Hot extremely dissolving, filters, and adds 200ml deionized water in filtrate, using the ultrasonic lucifuge process at 0～5 DEG C of 30khz
30min, stands still for crystals, and dries, obtain the rutin 18.77g of purity 98.27%, yield 23.46% at 130 DEG C.
Embodiment 3
120g is dried the Flos Sophorae Immaturus and is crushed to 50 mesh, add temperature to be 40 DEG C, after the sour water of ph=4～5, insert supercritical
co2In extraction equipment, process 30min at pressure 30mpa, 40 DEG C of temperature, be 0～5 DEG C using temperature afterwards, ph=4～5
Acid rinsing dries twice afterwards；Flos Sophorae Immaturus granule after drying adds 3% Borax, 1% na2so3With 30 times of 60～70% ethanol
In, adjust ph to 9～10 using sodium bicarbonate, add 0.45% tween 20 and 0.05% op-15,30khz, 40 DEG C
Under conditions of lucifuge ultrasonic extraction 25min, filter afterwards, filtrate lucifuge at 40 DEG C is standby；Filtering residue is again with above-mentioned same
Condition extract once, the filtrate obtaining merges with filtrate before, to merging after filtrate in add 5% activated carbon, keep away at 40 DEG C
Light stirs 10min, will filter the acidification of filtrate after carbon removal to ph=3～4, stands 30min, sucking filtration obtains rutin crude product；Rutin is thick
Product are placed in baking oven, dry to no alcohol taste at 40 DEG C, then are gradually heating to 130 DEG C of drying, and the rutin that is dried obtaining is added 3l
It is heated in n-butyl alcohol dissolving, filters, add 300ml deionized water in filtrate, ultrasonic using 30khz is kept away at 0～5 DEG C
Optical processing 25min, stands still for crystals and dries at 130 DEG C, obtain the rutin 28.22g of purity 98.35%, yield 23.52%.
Claims (4)
1. a kind of method of rutin of extracting from the Flos Sophorae Immaturus is it is characterised in that comprise the following steps:
(1) clean enzyme denaturing: it is crushed to 20～80 mesh by the Flos Sophorae Immaturus are dried, add temperature to be 30～40 DEG C, after the sour water of ph=4～5,
Insert supercritical co2In extraction equipment, pressure be 30mpa, temperature be 30～40 DEG C at process 20～40min, use afterwards
Temperature is 0～5 DEG C, and the acid rinsing of ph=4～5 dries twice afterwards；
(2) extract: the Flos Sophorae Immaturus granule after drying adds 1～5% Borax, 1～5% na2so3With the 60～70% of 15-30 times
In ethanol, adjust ph to 9～10 using sodium bicarbonate, add 0.35～0.45% tween 20 and 0.05～0.15%
op-15；Filter after ultrasonic extraction 15～25min under the conditions of 30khz, 40～50 DEG C, filtrate lucifuge at 30～50 DEG C
Standby；Filtering residue is extracted once with above-mentioned same condition again, and the filtrate obtaining is merged with filtrate before, the filtrate to after merge
Middle addition 5% activated carbon, lucifuge stirring 10min at 30～50 DEG C, will filter the acidification of filtrate after carbon removal to ph=3～4, stands
20～30min, sucking filtration obtains rutin crude product；
(3) refine: rutin crude product is placed in baking oven, dries to no alcohol taste at 40 DEG C, then be gradually heating to 130 DEG C of drying, will
Being dried in rutin addition n-butyl alcohol of obtaining is heated to dissolving, and filters, adds deionized water, using 20～30khz in filtrate
Ultrasonic at 0～5 DEG C lucifuge process 20～30min, stand still for crystals and at 130 DEG C dry, obtain purity 98% reach above
Rutin, yield reaches more than 23%.
2. as claimed in claim 1 a kind of extract rutin method it is characterised in that: in described step (1), destroy the enzyme treatment
Time is 40min；Described sour water is aqueous hydrochloric acid solution.
3. as claimed in claim 1 or 2 a kind of extract rutin method it is characterised in that: in described step (2), add 3～
4% Borax and 1% na2so3.
4. as claimed in claim 1 or 2 a kind of extract rutin method it is characterised in that: in described step (3), add just
The volume of butanol is 20～30ml/g with the ratio of Flos Sophorae Immaturus raw materials quality；Add the volume of deionized water and the ratio of Flos Sophorae Immaturus raw materials quality
For 2～3ml/g；Ultrasonic Treatment 20～30min under 30khz.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410390859.8A CN104098635B (en) | 2014-08-11 | 2014-08-11 | Method for extracting rutin from sophora flower bud |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410390859.8A CN104098635B (en) | 2014-08-11 | 2014-08-11 | Method for extracting rutin from sophora flower bud |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN104098635A CN104098635A (en) | 2014-10-15 |
| CN104098635B true CN104098635B (en) | 2017-02-01 |
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| CN201410390859.8A Active CN104098635B (en) | 2014-08-11 | 2014-08-11 | Method for extracting rutin from sophora flower bud |
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| CN104744535A (en) * | 2015-02-28 | 2015-07-01 | 天津理工大学 | Method for extracting rutin from leaves of Aralia elata var.inermis |
| 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 |
| CN106397513A (en) * | 2016-10-27 | 2017-02-15 | 广西禅方药业股份有限公司 | Method for refining rutin having content more than or equal to 98% |
| CN108623646A (en) * | 2018-07-09 | 2018-10-09 | 山东端信堂大禹药业有限公司 | A kind of device and its extracting method extracting rutin from the sophora bud |
| 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 |
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| RO99802B1 (en) * | 1988-04-11 | 1990-09-28 | Institutul De Cercetari Chimico-Farmaceutice | Process for extracting and purifying rutoside |
| CN102718820B (en) * | 2012-07-10 | 2013-07-03 | 刘志强 | Method for extracting and refining rutin |
| CN103435667A (en) * | 2013-09-17 | 2013-12-11 | 南京通泽农业科技有限公司 | Novel method for extracting rutin from pagodatree flower bud |
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