CN104098635A - Method for extracting rutin from sophora flower bud - Google Patents
Method for extracting rutin from sophora flower bud Download PDFInfo
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- CN104098635A CN104098635A CN201410390859.8A CN201410390859A CN104098635A CN 104098635 A CN104098635 A CN 104098635A CN 201410390859 A CN201410390859 A CN 201410390859A CN 104098635 A CN104098635 A CN 104098635A
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- rutin
- filtrate
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- sophora bud
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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 56
- 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 56
- 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 56
- 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 56
- 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 56
- 235000005493 rutin Nutrition 0.000 title claims abstract description 56
- 229960004555 rutoside Drugs 0.000 title claims abstract description 56
- 238000000034 method Methods 0.000 title claims abstract description 32
- 241000219784 Sophora Species 0.000 title claims abstract description 28
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 17
- 238000000605 extraction Methods 0.000 claims abstract description 14
- 102000004190 Enzymes Human genes 0.000 claims abstract description 13
- 108090000790 Enzymes Proteins 0.000 claims abstract description 13
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 claims abstract description 12
- 238000001035 drying Methods 0.000 claims abstract description 12
- 229920001213 Polysorbate 20 Polymers 0.000 claims abstract description 10
- 239000000256 polyoxyethylene sorbitan monolaurate Substances 0.000 claims abstract description 10
- 235000010486 polyoxyethylene sorbitan monolaurate Nutrition 0.000 claims abstract description 10
- 238000002425 crystallisation Methods 0.000 claims abstract description 8
- 230000008025 crystallization Effects 0.000 claims abstract description 8
- 238000001914 filtration Methods 0.000 claims abstract description 6
- 238000007670 refining Methods 0.000 claims abstract description 3
- 239000000706 filtrate Substances 0.000 claims description 31
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 20
- 230000008569 process Effects 0.000 claims description 13
- UIIMBOGNXHQVGW-UHFFFAOYSA-M Sodium bicarbonate Chemical compound [Na+].OC([O-])=O UIIMBOGNXHQVGW-UHFFFAOYSA-M 0.000 claims description 10
- 239000012043 crude product Substances 0.000 claims description 10
- 239000000284 extract Substances 0.000 claims description 10
- 239000008367 deionised water Substances 0.000 claims description 8
- 229910021641 deionized water Inorganic materials 0.000 claims description 8
- 238000002137 ultrasound extraction Methods 0.000 claims description 8
- 239000002253 acid Substances 0.000 claims description 7
- 229910021538 borax Inorganic materials 0.000 claims description 7
- 229910052708 sodium Inorganic materials 0.000 claims description 7
- 239000011734 sodium Substances 0.000 claims description 7
- 239000004328 sodium tetraborate Substances 0.000 claims description 7
- 235000010339 sodium tetraborate Nutrition 0.000 claims description 7
- 241000196324 Embryophyta Species 0.000 claims description 6
- 239000002994 raw material Substances 0.000 claims description 6
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 5
- 229910052799 carbon Inorganic materials 0.000 claims description 5
- 239000002245 particle Substances 0.000 claims description 5
- 229910000030 sodium bicarbonate Inorganic materials 0.000 claims description 5
- 235000017557 sodium bicarbonate Nutrition 0.000 claims description 5
- 238000003756 stirring Methods 0.000 claims description 5
- 238000000967 suction filtration Methods 0.000 claims description 5
- 238000010792 warming Methods 0.000 claims description 5
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 4
- 238000002525 ultrasonication Methods 0.000 claims description 3
- 238000004519 manufacturing process Methods 0.000 abstract description 3
- 238000005406 washing Methods 0.000 abstract description 3
- 239000004094 surface-active agent Substances 0.000 abstract description 2
- 230000009849 deactivation Effects 0.000 abstract 1
- 239000007788 liquid Substances 0.000 abstract 1
- 239000013543 active substance Substances 0.000 description 5
- 239000000126 substance Substances 0.000 description 4
- 239000003814 drug Substances 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 238000002386 leaching Methods 0.000 description 3
- 230000003647 oxidation Effects 0.000 description 3
- 238000007254 oxidation reaction Methods 0.000 description 3
- 238000007664 blowing Methods 0.000 description 2
- 239000000470 constituent Substances 0.000 description 2
- 235000013305 food Nutrition 0.000 description 2
- 238000004128 high performance liquid chromatography Methods 0.000 description 2
- 230000007062 hydrolysis Effects 0.000 description 2
- 238000006460 hydrolysis reaction Methods 0.000 description 2
- 238000005457 optimization Methods 0.000 description 2
- 238000011282 treatment Methods 0.000 description 2
- 208000007530 Essential hypertension Diseases 0.000 description 1
- 208000032843 Hemorrhage Diseases 0.000 description 1
- 208000031226 Hyperlipidaemia Diseases 0.000 description 1
- 208000004880 Polyuria Diseases 0.000 description 1
- 244000046101 Sophora japonica Species 0.000 description 1
- 235000010586 Sophora japonica Nutrition 0.000 description 1
- 238000004220 aggregation Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 229930013930 alkaloid Natural products 0.000 description 1
- 150000003797 alkaloid derivatives Chemical class 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
- 239000007864 aqueous solution Substances 0.000 description 1
- 230000004856 capillary permeability Effects 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000007795 chemical reaction product Substances 0.000 description 1
- 239000000084 colloidal system Substances 0.000 description 1
- 239000002537 cosmetic Substances 0.000 description 1
- 206010012601 diabetes mellitus Diseases 0.000 description 1
- 230000035619 diuresis Effects 0.000 description 1
- 230000007613 environmental effect Effects 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
- 210000003677 hemocyte Anatomy 0.000 description 1
- 229940000351 hemocyte Drugs 0.000 description 1
- 206010020718 hyperplasia Diseases 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 230000000415 inactivating effect Effects 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 150000002632 lipids Chemical class 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 230000002265 prevention Effects 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 238000010298 pulverizing process Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 238000004904 shortening Methods 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 238000002560 therapeutic procedure Methods 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
Abstract
The invention discloses a novel 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 relates to a kind of method of extracting rutin from the sophora bud.
Background technology
The sophora bud is the dry flower and alabastrum of leguminous plants Chinese scholartree, the history of being used as medicine existing more than 2000 year, and Shennong's Herbal is classified as top grade.The rutin containing in the sophora bud claims again violaguercitrin, rutin, belong to flavonoid glycoside compound, can reduce capillary permeability and fragility, promote hyperplasia and prevent that hemocyte from condensing, also have anti-inflammatory, antianaphylaxis, diuresis, antibechic, reducing blood-fat etc. effect.Rutin clinically as the assisting therapy of essential hypertension, prevent because rutin lacks other hemorrhages that cause and prevention and treatment diabetes and merging hyperlipidemia.In addition, rutin is as natural antioxidant and use yellow pigment, is also widely used in protective foods and cosmetic kind.Rutin, in sophora bud airing, washing, pulverizing, leaching process, is vulnerable to coexist in the rue enzyme effect in the sophora bud and is hydrolyzed, and therefore, enzyme or to reduce the activity of enzyme very important goes out before extracting or in leaching process.The enzyme inactivating method of available technology adopting mainly contain dry blowing, uviolizing,
60co irradiation, microwave deactivating enzyme etc., wherein dry blowing temperature is high, can cause hydrolysis and the oxidation of rutin in the enzyme that goes out, and also can cause part rutin be dissolved in hot water and run off; Though and the uviolizing enzyme that can effectively go out, the used time is longer, cost is also high, and production efficiency is reduced.Along with tensio-active agent being widely used in fields such as chemical industry, food, daily necessities production and water treatments, water insoluble or not soluble in water effective constituent in a lot of Chinese medicine, as Flavonoid substances, alkaloid, volatilization wet goods, can on its surface or interface, form adsorption by tensio-active agent, or in solution, form molecule aggregation body, and then change the solvability of these compositions in the aqueous solution, improve the extraction efficiency of Chinese medicine, reduce extraction cost, the feature of safety and environmental protection.
In prior art, there is the report that adopts the auxiliary Extraction of rutin of tensio-active agent, but adopt a kind of tensio-active agent more.As (" the improvement researchs of Rutin Extracting Technology " such as Li Jinxiu, Li Jinxiu, Gong Shengzhao, Huang Qiujin, Guangdong chemical industry, the 1st phase in 2003, P15) adopted following methods to carry out the extraction of violaguercitrin: the sophora bud is pulverized, add the water of 5 times of amounts, regulate pH8～9 with liming, be 50～60 DEG C in temperature and extract 20～30min, filter, repeatedly extract 3 times by similarity condition, filtrate is 3 with salt acid for adjusting pH, add 0.5% Surfactant OP, at 60～70 DEG C of insulation 10min, leave standstill 30min, filter, washing, dry, obtain violaguercitrin product yield 18.4%, content 96%.
Summary of the invention
The application aims to provide a kind of new method of extracting rutin from the sophora bud.
The method of the invention comprises the following steps:
(1) clean the enzyme that goes out: will be dried the sophora bud and be crushed to 20～80 orders, adding temperature is 30～40 DEG C, after the sour water of pH=4～5, inserts supercritical CO
2in extraction plant, be that 30MPa, temperature are to process 20～40min at 30～40 DEG C at pressure, use temperature is 0～5 DEG C afterwards, twice rear drying of acid rinsing of pH=4～5;
(2) extract: the sophora bud particle after drying adds 1～5% borax, 1～5% Na
2sO
3in 15-30 60～70% ethanol doubly, use sodium bicarbonate to regulate pH to 9～10, add again the OP-15 of 0.3～0.4% Tween 20 and 0.05～0.2%, lucifuge ultrasonic extraction 10～30min under 20～30kHz, the condition of 30～50 DEG C, filter afterwards, filtrate lucifuge at 30～50 DEG C is for subsequent use; Filter residue extracts once with above-mentioned same condition again, and the filtrate obtaining merges with filtrate before, in the filtrate after merging, adds 5% gac, at 30～50 DEG C, lucifuge stirs 10min, the filtrate of filtering after carbon removal is acidified to pH=3～4, leaves standstill 20～30min, suction filtration obtains rutin crude product;
(3) refining: rutin crude product is placed in to baking oven, at 40 DEG C, dry extremely without alcohol taste, be warming up to gradually again 130 DEG C of oven dry, the dry rutin obtaining is added in propyl carbinol and is heated to dissolve, filter, in filtrate, add deionized water, adopt 20～30kHz ultrasonic lucifuge at 0～5 DEG C to process 20～30min, leave standstill crystallization and dry at 130 DEG C, obtaining purity 98% and reach above rutin, yield reaches more than 23%.
Further, in step of the present invention (1), the preferred 40min of time of the enzyme processing of going out; Described sour water can be aqueous hydrochloric acid.
Further, in step of the present invention (2), preferably add 3～4% borax and 1% Na
2sO
3.
Further, in step of the present invention (2), preferably add the OP-15 of 0.35～0.45% Tween 20 and 0.05～0.15%.
Further, in step of the present invention (2), the condition optimization of ultrasonic extraction extracts 15～25min at 30kHz, 40～50 DEG C;
Further, in step of the present invention (3), adding the volume of propyl carbinol and the ratio of sophora bud raw materials quality is 20～30mL/g; Adding the volume of deionized water and the ratio of sophora bud raw materials quality is 2～3mL/g; The condition optimization of ultrasonication is processed 20～30min under 30 kHz.
The present invention adopts supercritical CO
2the enzyme that goes out, the used time is short, and rutin is at supercritical CO
2not soluble under condition, can not cause hydrolysis, oxidation and the loss of rutin, retain to greatest extent the active constituent content of rutin; The tensio-active agent Tween 20 of rational proportion and OP-15 make extraction time and crystallization time all have shortening, and extraction efficiency improves, then is aided with ultrasonic wave, and the oxidation wastage of rutin in leaching process reduced, and yield increases obviously.Adopt propyl carbinol to refine rutin, can effectively remove the impurity such as residual colloid, lipid acid, improve the purity of rutin.Comprehensive each step of the present invention, the method for the invention is easy and simple to handle, and extraction efficiency is high, is applicable to produce actual.
Brief description of the drawings
Fig. 1 is rutin standard substance HPLC spectrogram.
Fig. 2 is the HPLC spectrogram of rutin end product in embodiment 2.
Embodiment
Embodiment 1
The dry 50g sophora bud is crushed to 40 orders, and adding temperature is, after 40 DEG C, the sour water of pH=4～5, to insert supercritical CO
2in extraction plant, at 40 DEG C of pressure 30MPa, temperature, process 20～40min, use temperature is 0～5 DEG C afterwards, twice rear drying of acid rinsing of pH=4～5; Sophora bud particle after drying adds 3% borax, 1% Na
2sO
3in 60% ethanol of 25 times, use sodium bicarbonate to regulate pH to 9～10, then add 0.35% Tween 20 and 0.15% OP-15, lucifuge ultrasonic extraction 20min under 30kHz, the condition of 40 DEG C, filters afterwards, and filtrate lucifuge at 40 DEG C is for subsequent use; Filter residue extracts once with above-mentioned same condition again, and the filtrate obtaining merges with filtrate before, in the filtrate after merging, adds 5% gac, at 40 DEG C, lucifuge stirs 10min, the filtrate of filtering after carbon removal is acidified to pH=3～4, leaves standstill 20min, suction filtration obtains rutin crude product; Rutin crude product is placed in to baking oven, at 40 DEG C, dry extremely without alcohol taste, be warming up to gradually again 130 DEG C of oven dry, the dry rutin obtaining is added in 1300mL propyl carbinol and is heated to dissolve, filter, in filtrate, add 130mL deionized water, adopt 30kHz ultrasonic lucifuge at 0～5 DEG C to process 20min, leave standstill crystallization, dry at 130 DEG C, obtain the rutin 11.61g of purity 98.33%, yield 23.21%.
Embodiment 2
The dry 80g sophora bud is crushed to 50 orders, and adding temperature is, after 40 DEG C, the sour water of pH=4～5, to insert supercritical CO
2in extraction plant, at 40 DEG C of pressure 30MPa, temperature, process 30min, use temperature is 4 DEG C afterwards, twice rear drying of acid rinsing of pH=4～5; Sophora bud particle after drying adds 4% borax, 1% Na
2sO
3in 70% ethanol of 20 times, use sodium bicarbonate to regulate pH to 9～10, then add 0.4% Tween 20 and 0.1% OP-15, lucifuge ultrasonic extraction 25min under 30kHz, the condition of 40 DEG C, filters afterwards, and filtrate lucifuge at 40 DEG C is for subsequent use; Filter residue extracts once with above-mentioned same condition again, and the filtrate obtaining merges with filtrate before, in the filtrate after merging, adds 5% gac, at 40 DEG C, lucifuge stirs 10min, the filtrate of filtering after carbon removal is acidified to pH=3～4, leaves standstill 25min, suction filtration obtains rutin crude product; Rutin crude product is placed in to baking oven, at 40 DEG C, dry extremely without alcohol taste, be warming up to gradually again 130 DEG C of oven dry, the dry rutin obtaining is added in 2L propyl carbinol and is heated to dissolve, filter, in filtrate, add 200mL deionized water, adopt 30kHz ultrasonic lucifuge at 0～5 DEG C to process 30min, leave standstill crystallization, dry at 130 DEG C, obtain the rutin 18.77g of purity 98.27%, yield 23.46%.
Embodiment 3
The dry 120g sophora bud is crushed to 50 orders, and adding temperature is, after 40 DEG C, the sour water of pH=4～5, to insert supercritical CO
2in extraction plant, at 40 DEG C of pressure 30MPa, temperature, process 30min, use temperature is 0～5 DEG C afterwards, twice rear drying of acid rinsing of pH=4～5; Sophora bud particle after drying adds 3% borax, 1% Na
2sO
3in 60～70% ethanol of 30 times, use sodium bicarbonate to regulate pH to 9～10, then add 0.45% Tween 20 and 0.05% OP-15, lucifuge ultrasonic extraction 25min under 30kHz, the condition of 40 DEG C, filters afterwards, and filtrate lucifuge at 40 DEG C is for subsequent use; Filter residue extracts once with above-mentioned same condition again, and the filtrate obtaining merges with filtrate before, in the filtrate after merging, adds 5% gac, at 40 DEG C, lucifuge stirs 10min, the filtrate of filtering after carbon removal is acidified to pH=3～4, leaves standstill 30min, suction filtration obtains rutin crude product; Rutin crude product is placed in to baking oven, at 40 DEG C, dry extremely without alcohol taste, be warming up to gradually again 130 DEG C of oven dry, the dry rutin obtaining is added in 3L propyl carbinol and is heated to dissolve, filter, in filtrate, add 300mL deionized water, adopt 30kHz ultrasonic lucifuge at 0～5 DEG C to process 25min, leave standstill crystallization and dry at 130 DEG C, obtaining the rutin 28.22g of purity 98.35%, yield 23.52%.
Claims (8)
1. a method of extracting rutin from the sophora bud, is characterized in that comprising the following steps:
(1) clean the enzyme that goes out: will be dried the sophora bud and be crushed to 20～80 orders, adding temperature is 30～40 DEG C, after the sour water of pH=4～5, inserts supercritical CO
2in extraction plant, be that 30MPa, temperature are to process 20～40min at 30～40 DEG C at pressure, use temperature is 0～5 DEG C afterwards, twice rear drying of acid rinsing of pH=4～5;
(2) extract: the sophora bud particle after drying adds 1～5% borax, 1～5% Na
2sO
3in 15-30 60～70% ethanol doubly, use sodium bicarbonate to regulate pH to 9～10, add again the OP-15 of 0.3～0.5% Tween 20 and 0.05～0.2%, lucifuge ultrasonic extraction 10～30min under 20～30kHz, the condition of 30～50 DEG C, filter afterwards, filtrate lucifuge at 30～50 DEG C is for subsequent use; Filter residue extracts once with above-mentioned same condition again, and the filtrate obtaining merges with filtrate before, in the filtrate after merging, adds 5% gac, at 30～50 DEG C, lucifuge stirs 10min, the filtrate of filtering after carbon removal is acidified to pH=3～4, leaves standstill 20～30min, suction filtration obtains rutin crude product;
(3) refining: rutin crude product is placed in to baking oven, at 40 DEG C, dry extremely without alcohol taste, be warming up to gradually again 130 DEG C of oven dry, the dry rutin obtaining is added in propyl carbinol and is heated to dissolve, filter, in filtrate, add deionized water, adopt 20～30kHz ultrasonic lucifuge at 0～5 DEG C to process 20～30min, leave standstill crystallization and dry at 130 DEG C, obtaining purity 98% and reach above rutin, yield reaches more than 23%.
2. a kind of method of extracting rutin as claimed in claim 1, is characterized in that: in described step (1), the time of the enzyme processing of going out is 40min; Described sour water can be aqueous hydrochloric acid.
3. a kind of method of extracting rutin as claimed in claim 1 or 2, is characterized in that: in described step (2), add 3～4% borax and 1% Na
2sO
3.
4. a kind of method of extracting rutin as claimed in claim 1 or 2, is characterized in that: in described step (2), add the OP-15 of 0.35～0.45% Tween 20 and 0.05～0.15%.
5. a kind of method of extracting rutin as claimed in claim 1 or 2, is characterized in that: in described step (2), and ultrasonic extraction 15～25min under 30kHz, 40～50 DEG C of conditions.
6. a kind of method of extracting rutin as claimed in claim 1 or 2, is characterized in that: in described step (3), adding the volume of propyl carbinol and the ratio of sophora bud raw materials quality is 20～30mL/g; Adding the volume of deionized water and the ratio of sophora bud raw materials quality is 2～3mL/g; Ultrasonication 20～30min under 30 kHz.
7. a kind of method of extracting rutin as claimed in claim 3, is characterized in that: in described step (2), add the OP-15 of 0.35～0.45% Tween 20 and 0.05～0.15%; Ultrasonic extraction 15～25min under 30kHz, 40～50 DEG C of conditions.
8. a kind of method of extracting rutin as claimed in claim 7, is characterized in that: in described step (3), adding the volume of propyl carbinol and the ratio of sophora bud raw materials quality is 20～30mL/g; Adding the volume of deionized water and the ratio of sophora bud raw materials quality is 2～3mL/g; Ultrasonication 20～30min under 30 kHz.
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| CN201410390859.8A CN104098635B (en) | 2014-08-11 | 2014-08-11 | Method for extracting rutin from sophora flower bud |
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| CN201410390859.8A CN104098635B (en) | 2014-08-11 | 2014-08-11 | Method for extracting rutin from sophora flower bud |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| RO99802B1 (en) * | 1988-04-11 | 1990-09-28 | Institutul De Cercetari Chimico-Farmaceutice | Process for extracting and purifying rutoside |
| CN102718820A (en) * | 2012-07-10 | 2012-10-10 | 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 |
-
2014
- 2014-08-11 CN CN201410390859.8A patent/CN104098635B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| RO99802B1 (en) * | 1988-04-11 | 1990-09-28 | Institutul De Cercetari Chimico-Farmaceutice | Process for extracting and purifying rutoside |
| CN102718820A (en) * | 2012-07-10 | 2012-10-10 | 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 |
Non-Patent Citations (4)
| Title |
|---|
| 张德权，等: "《食品超临界CO2流体加工技术》", 31 May 2005, article "超临界非酶反应技术在食品工业中的应用", pages: 211-215 * |
| 银建中，等: "槐花浸膏和芦丁的超临界CO2提纯工艺研究", 《医药工程设计》, vol. 27, no. 6, 31 December 2006 (2006-12-31), pages 2 - 3 * |
| 马国刚: "槐米芦丁的超声波辅助提取及化学修饰研究", 《北京林业大学硕士学位论文》, 15 January 2009 (2009-01-15), pages 14 - 33 * |
| 龚盛昭，等: "表面活性剂协同提取芦丁研究", 《林产化学与工业》, vol. 24, 31 August 2004 (2004-08-31), pages 96 * |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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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