CN101665479B - Technology for synchronously extracting isofraxidin and flavonoids compounds from sarcandra glabra and applications thereof - Google Patents
Technology for synchronously extracting isofraxidin and flavonoids compounds from sarcandra glabra and applications thereof Download PDFInfo
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Abstract
The invention provides a technology for synchronously extracting isofraxidin and flavonoids compounds from sarcandra glabra and applications thereof, solving the problems that the prior art can not synchronously extract and separate isofraxidin and flavonoids compounds from sarcandra glabra, has low product purity and low productivity and the like. The technology adopts flat turning countercurrent extraction, obtains liquid extract by a climbing-film concentration evaporator and vacuum concentration, extracts the liquid extract and collects the liquid supernatant, crystallizes the liquid supernatant after concentration, adds silica gel for adsorption after the crystal is dissolved, crystallizes the mixture at low temperature, and obtains the high-purity isofraxidin after vacuum drying; the liquid extract sedimentation is dissolved by adopting alkaline ethanol solution and then centrifugalized to collect the sedimentation, and the sedimentation is dissolved by water, crystallized, separated and vacuum-dried to obtain the flavonoids compounds. The technology realizes the synchronous high-efficiency extract and separation of high-purity isofraxidin and flavonoids compounds, and has certain meaning and remarkable economic benefit on the wide application in the fields such as medicines, health care, make ups and the like.
Description
Technical field
The invention belongs to the Herba Pileae Scriptae extract technical field, more specifically relate to a kind of technology and application of simultaneous extraction isofraxidin and flavonoid compound from Herba Pileae Scriptae.
Background technology
Herba Pileae Scriptae is planted another name nine joint flowers, Herba Pileae Scriptae, synthetism lotus, sarcandra glaber etc., its medicinal part herb, and flavor is hot, bitter, and property is flat.Have Azelaic Acid, clearing heat and detoxicating, dispel rheumatism, effect such as promoting blood circulation and stopping pain, the synthetism of stimulating the menstrual flow, be used to treat various diseases associated with inflammation, rheumatic arthritis, sore swollen toxin, wound, fracture etc.In recent years being used to treat carcinoma of the pancreas, cancer of the stomach, the rectum cancer, liver cancer, esophagus cancer etc. has than unusual effect.Herba Pileae Scriptae is widely used in fields such as medicine, health care, daily cosmetics because of its unique medicinal efficacy, and market demand is cumulative year after year trend.
The content of isofraxidin is about 0.03% in the Herba Pileae Scriptae, and the content in Herba Pileae Scriptae is higher, is one of main effective constituent of Herba Pileae Scriptae; Except having antibiotic significantly, antitumous effect; Also the immune system of adjustable skin and mucous membrane improves the resistibility of skin film, and relaxes the stimulation of exterior materials to skin; Can treat the skin function disorders, as skin examine, eczema etc.In makeup, then can be used as amendment, oxidation-resistance is also arranged, can prevent the oxidation of lipid.The Herba Pileae Scriptae flavones is owing to the existence of the phenolic hydroxyl group on the phenyl ring, its anti-inflammatory, sterilization; Clearing heat and detoxicating, the pharmacology of anti-kinds of tumors just is understood that, and relevant report shows; Herba Pileae Scriptae all has inhibitory or killing effect to streptococcus aureus and dysentery, typhoid fever, intestinal bacteria etc., so sarcandra glabra fluid extract except that the application aspect toothpaste, also can be used as a kind of Chinese medicine additive; Be used for some functional makeup, like body wash etc.
But because the separating difficulty that from Herba Pileae Scriptae, extracts isofraxidin and flavonoid compound so related prods is directly used with Herba Pileae Scriptae crude drug or medicinal extract basically on the current market, thereby has also limited its Application Areas than higher.
Summary of the invention
The present invention provides a kind of technology and application of simultaneous extraction isofraxidin and flavonoid compound from Herba Pileae Scriptae; Solve in the prior art extraction separation isofraxidin and flavonoid compound from Herba Pileae Scriptae simultaneously; Problems such as isolating product purity is not high, and productive rate is low; The high-level efficiency extraction separation has certain significance to it in extensive applications such as medicine, health care, daily cosmetics when realizing while high purity isofraxidin and flavonoid compound.
The technology of simultaneous extraction isofraxidin and flavonoid compound from Herba Pileae Scriptae: adopt the hoirzontally rotating countercurrent extraction, the membrane-concentrated vaporizer concentrates through rising, vacuum concentration, obtains fluid extract; Extract fluid extract 3-5 time; Collect supernatant, with the supernatant concentration post crystallization, with going up silica gel adsorption behind the dissolution of crystals; Low temperature crystallization behind the wash-out obtains the high purity isofraxidin after the vacuum-drying; Extraction is placed spinning after 24-48 hour after collecting the fluid extract deposition employing alkaline ethanol solution dissolving after the supernatant, and collecting precipitation will precipitate and use water dissolution, crystallization, and spinning again, vacuum-drying obtains flavonoid compound.
Isofraxidin of the present invention and flavonoid compound can be widely used in preparation medicine, healthcare products or makeup.
Remarkable advantage of the present invention is: the present invention adopts hoirzontally rotating countercurrent extraction method to combine to extract vacuum concentration, can improve the extraction yield of isofraxidin and flavonoid compound greatly, has guaranteed the quality of two kinds of products; And improved the solvent recuperation utilization ratio, and significantly reduced extraction cost, extract and isolate isofraxidin and flavonoid compound simultaneously; Practiced thrift extraction time, specifically the high purity isofraxidin of the present invention's preparation is a white crystalline powder, can not change original color during application; Both content is higher; Specific aim is stronger, and drug effect is better, with respect to Herba Pileae Scriptae crude drug, medicinal extract and so on; Application at aspects such as medicine, healthcare products, makeup is more extensive, has remarkable economic efficiency.
Embodiment
(1) the Herba Pileae Scriptae medicinal material is ground into 2-5cm before adopting the hoirzontally rotating countercurrent extraction.
(2) adopt the hoirzontally rotating countercurrent extraction; Rising the membrane-concentrated vaporizer concentrates: adopting in the said hoirzontally rotating countercurrent extraction method and extracting solvent is one or more mixed solvents in water, methyl alcohol, ethanol or the Virahol; The extraction solvent quality is that the 3-10 of Herba Pileae Scriptae quality of medicinal material doubly measures, and extracting temperature is 30-80 ℃, and extraction time is 3-5 time; Each extraction time is 1-5 hour, and the extracting solution flow is 15L/min.
(3) vacuum concentration; Obtain fluid extract: the solvent that extracts fluid extract is one or more mixed solvents in chloroform, methylene dichloride, sherwood oil, normal hexane or the solvent oil; Extracting solvent and fluid extract mass ratio is 3: 1-10: 1; Extraction time is 3-5 time, collects supernatant (the fluid extract deposition after the collection supernatant is subsequent use), is concentrated into the 5-20% of original volume; Recrystallization under the room temperature.
(4) with going up silica gel adsorption behind the dissolution of crystals; Wash-out: the crystal of recrystallization is with one or more the mixed solvent dissolving in methyl alcohol, ethanol, chloroform, methylene dichloride, sherwood oil, normal hexane or the solvent oil; The mass ratio 1 of crystal and elutriant: 1-1: 8; Last silicagel column absorption, used silica gel order number is the 20-200 order, the elutriant of employing is a kind of or its arbitrary proportion mixed solvent in sherwood oil, normal hexane, solvent oil or the ETHYLE ACETATE; Carry out wash-out, adopt the tlc contrast to collecting fully.
(5) low temperature crystallization; Obtain the high purity isofraxidin after the vacuum-drying: the crystal elutriant behind process silica gel adsorption, the wash-out is concentrated into the 5-20% of original volume, low temperature crystallization, and Tc is-10～10 ℃; Crystallization time is 5-24 hour, the one or many recrystallization.
Extraction is placed spinning after 24-48 hour after collecting the fluid extract deposition employing alkaline ethanol solution dissolving after the supernatant, and collecting precipitation will precipitate and use water dissolution, crystallization, and spinning again, vacuum-drying obtains flavonoid compound.
When extracting flavonoid compound, the fluid extract deposition is 1 with the mass ratio of alkaline ethanol solution: 1-1: 5; When deposition after the spinning is used water dissolution deposition and water mass ratio be 1: 1-1: 8;-30-0 ℃ of crystallization, time 12-48 hour, one or many recrystallization; Alcohol concn is 10-30wt% in the said alkaline ethanol solution, and (alkali of adding or alkaline, inorganic salts are conventional, like NaOH, KOH, Na to add alkali or alkaline, inorganic salts
2CO
3, NaHCO
3, K
2CO
3, KHCO
3Or the like in one or more) make its pH value for 8-12.
The present invention prepares the gained isofraxidin amount of containing ≧ 90%, and the rate of transform is greater than 60%, flavones kind compound content ≧ 95%, and the rate of transform is greater than 80%.
Isofraxidin and flavonoid compound according to above step preparation can be widely used in preparation medicine, healthcare products or makeup.
Below be several specific embodiment of the present invention, further specify the present invention, but the present invention be not limited only to this.
Embodiment 1
With every section of Herba Pileae Scriptae medicinal material chopping 2cm, adopt the hoirzontally rotating countercurrent extractor to extract with the methyl alcohol of 8 times of amounts 50%, the extraction temperature is controlled at 50 ℃, the extracting solution flow is 15L/min, accomplishes 3 times counter-current extraction, extraction time 3 hours/inferior.United extraction liquid, employing earlier rises the membrane-concentrated vaporizer and concentrates, and adopts vacuum concentration again, obtains fluid extract.Medicinal extract is collected supernatant with the chloroform extraction of 3 times of amounts three times, concentrates post crystallization, precipitates subsequent use.Crystal is with the dissolve with ethanol of 3 times of amounts, and eluent ethyl acetate use in last silicagel column absorption, and the collection elutriant is concentrated into 10% of original volume, crystallisation by cooling, and centrifugal, separation, vacuum-drying, gained isofraxidin content is 91.3%, the rate of transform 62.6%.It is 9 the aqueous ethanolic solution dissolving that contains alcohol concn 10wt% that above-mentioned deposition is used PH, places 24 hours, and centrifugal, collecting precipitation will precipitate and use water dissolution, crystallization, and spinning with crystallization vacuum-drying, obtains the Herba Pileae Scriptae flavones, content 95.2%, the rate of transform 86.3%.
Embodiment 2
The Herba Pileae Scriptae medicinal material is chopped into 5cm, adopts the hoirzontally rotating countercurrent extractor to extract, extract solvent and adopt 5 times of aqueous ethanolic solutions that mass concentration is 90wt%; Extract temperature and be controlled at 60 ℃; The extracting solution flow is 15L/min, accomplishes 2 times counter-current extraction, extraction time 5 hours/inferior.United extraction liquid, employing earlier rises the membrane-concentrated vaporizer and concentrates, and adopts vacuum concentration again, obtains fluid extract.Medicinal extract is collected supernatant (the medicinal extract deposition is subsequent use) and is concentrated post crystallization with the normal hexane extraction of 5 times of quality three times, and crystal is measured dissolve with methanol with 2 times; Last silicagel column absorption with normal hexane-ethyl acetate mixture (mass ratio of normal hexane-ETHYLE ACETATE is 10: 1) wash-out, is collected elutriant; Be concentrated into 10% of original volume, crystallisation by cooling, centrifugal, separation, vacuum-drying; Gained isofraxidin content is 92.6%, the rate of transform 64.5%.It is 10 the aqueous ethanolic solution dissolving that contains alcohol concn 20wt% that above-mentioned deposition is used PH, places 48 hours, and centrifugal, collecting precipitation will precipitate and use water dissolution, crystallization, and spinning with crystallization vacuum-drying, obtains the Herba Pileae Scriptae flavones, content 96.5%, the rate of transform 86.5%.
Embodiment 3
(1) the Herba Pileae Scriptae medicinal material is ground into 3cm before adopting the hoirzontally rotating countercurrent extraction.
(2) adopt the hoirzontally rotating countercurrent extraction; Rising the membrane-concentrated vaporizer concentrates: adopting in the said hoirzontally rotating countercurrent extraction method and extracting solvent is water; Extracting solvent quality is 10 times of amounts of Herba Pileae Scriptae quality of medicinal material, and extracting temperature is 80 ℃, and extraction time is 5 times; Each extraction time is 5 hours, and the extracting solution flow is 15L/min.
(3) vacuum concentration obtains fluid extract: the solvent that extracts fluid extract is a methylene dichloride, and extracting solvent and fluid extract mass ratio is 3: 1, and extraction time is 3 times, collects supernatant (the fluid extract deposition after the collection supernatant is subsequent use), is concentrated into 5% of original volume; Recrystallization under the room temperature.
(4) with going up silica gel adsorption, wash-out behind the dissolution of crystals: the crystal of recrystallization is with 3 times of amount petroleum ether dissolutions, and last silicagel column adsorbs, and used silica gel order number is 20 orders, and the elutriant of employing is a sherwood oil, carries out wash-out, adopts the tlc contrast complete to collecting.
(5) low temperature crystallization obtains the high purity isofraxidin after the vacuum-drying: the crystal elutriant through behind silica gel adsorption, the wash-out is concentrated into 5% of original volume, low temperature crystallization, and Tc is-10～-5 ℃, crystallization time is 5-8 hour, the one or many recrystallization.
Extraction is placed spinning after 24 hours after collecting the fluid extract deposition employing alkaline ethanol solution dissolving after the supernatant, and collecting precipitation will precipitate and use water dissolution, crystallization, and spinning again, vacuum-drying obtains flavonoid compound.
When extracting flavonoid compound, the fluid extract deposition is 1: 1 with the mass ratio of alkaline ethanol solution; When deposition after the spinning is used water dissolution deposition and water mass ratio be 1: 1;-30 ℃ of crystallizations, 12 hours time, primary crystallization; Alcohol concn is 15wt% in the said alkaline ethanol solution, and (alkali of adding or alkaline, inorganic salts are conventional, like NaOH, KOH, Na to add alkali or alkaline, inorganic salts
2CO
3, NaHCO
3, K
2CO
3, KHCO
3Or the like in one or more) to make its pH value be 10 (as incorrect, please revise).Preparation gained isofraxidin content 92.3%, the rate of transform 63.2%, flavonoid content 93.4%, the rate of transform 84.5%.
Embodiment 4
(1) the Herba Pileae Scriptae medicinal material is ground into 4cm before adopting the hoirzontally rotating countercurrent extraction.
(2) adopt the hoirzontally rotating countercurrent extraction; Rising the membrane-concentrated vaporizer concentrates: adopting in the said hoirzontally rotating countercurrent extraction method and extracting solvent is Virahol; Extracting solvent quality is 3 times of amounts of Herba Pileae Scriptae quality of medicinal material, and extracting temperature is 30 ℃, and extraction time is 3 times; Each extraction time is 1 hour, and the extracting solution flow is 15L/min.
(3) vacuum concentration; Obtain fluid extract: the solvent that extracts fluid extract is the mixed solvent of one or both any ratios in sherwood oil or the normal hexane; Extracting solvent and fluid extract mass ratio is 10: 1; Extraction time is 3 times, collects supernatant (the fluid extract deposition after the collection supernatant is subsequent use), is concentrated into 20% of original volume; Recrystallization under the room temperature.
(4) with going up silica gel adsorption behind the dissolution of crystals; Wash-out: the crystal of recrystallization with in chloroform, methylene dichloride or the solvent oil one or more arbitrarily than mixed solvent dissolving, the mass ratio of crystal and elutriant 1: 1, last silicagel column adsorbs; Used silica gel order number is 200 orders; The elutriant that adopts is a kind of or its two kinds the arbitrary proportion mixed solvent in normal hexane or the ETHYLE ACETATE, carries out wash-out, adopts the tlc contrast to collecting fully.
(5) low temperature crystallization obtains the high purity isofraxidin after the vacuum-drying: the crystal elutriant through behind silica gel adsorption, the wash-out is concentrated into 20% of original volume, low temperature crystallization, and Tc is 10 ℃, crystallization time is 24 hours, the one or many recrystallization.
Extraction is placed spinning after 48 hours after collecting the fluid extract deposition employing alkaline ethanol solution dissolving after the supernatant, and collecting precipitation will precipitate and use water dissolution, crystallization, and spinning again, vacuum-drying obtains flavonoid compound.
When extracting flavonoid compound, the fluid extract deposition is 1: 5 with the mass ratio of alkaline ethanol solution; When deposition after the spinning is used water dissolution deposition and water mass ratio be 1: 8; 0 ℃ of crystallization, time 48 hours, 3-5 time recrystallization; Alcohol concn is 15wt% in the said alkaline ethanol solution, and (alkali of adding or alkaline, inorganic salts are conventional, like NaOH, KOH, Na to add alkali or alkaline, inorganic salts
2CO
3, NaHCO
3, K
2CO
3, KHCO
3Or the like in one or more) to make its pH value be 10.The present invention prepares gained isofraxidin content 95.3%, the rate of transform 80.4%, flavonoid content 98.7%, the rate of transform 89.2%.
Preparation gained isofraxidin content 92.3%, the rate of transform 68.5%, flavonoid content 93.4%, the rate of transform 81.4%.
Embodiment 5
(1) the Herba Pileae Scriptae medicinal material is ground into 3-4cm before adopting the hoirzontally rotating countercurrent extraction.
(2) adopt the hoirzontally rotating countercurrent extraction; Rising the membrane-concentrated vaporizer concentrates: adopt in the said hoirzontally rotating countercurrent extraction method extract solvent be in ethanol or the Virahol one or both arbitrarily than mixed solvent; Extracting solvent quality is 6 times of amounts of Herba Pileae Scriptae quality of medicinal material, and extracting temperature is 70 ℃, and extraction time is 4 times; Each extraction time is 2 hours, and the extracting solution flow is 15L/min.
(3) vacuum concentration obtains fluid extract: the solvent that extracts fluid extract is a sherwood oil, and extracting solvent and fluid extract mass ratio is 5: 1, and extraction time is 4 times, collects supernatant (the fluid extract deposition after the collection supernatant is subsequent use), is concentrated into 10% of original volume; Recrystallization under the room temperature.
(4) with going up silica gel adsorption behind the dissolution of crystals; Wash-out: the crystal of recrystallization is used n-hexane dissolution, the mass ratio of crystal and elutriant 1: 3, last silicagel column absorption; Used silica gel order number is 100 orders; The elutriant that adopts is a kind of or its arbitrary proportion mixed solvent in sherwood oil, normal hexane, solvent oil or the ETHYLE ACETATE, carries out wash-out, adopts the tlc contrast to collecting fully.
(5) low temperature crystallization obtains the high purity isofraxidin after the vacuum-drying: the crystal elutriant through behind silica gel adsorption, the wash-out is concentrated into 10% of original volume, low temperature crystallization, and Tc is 5 ℃, crystallization time is 15 hours, the one or many recrystallization.
Extraction is placed spinning after 36 hours after collecting the fluid extract deposition employing alkaline ethanol solution dissolving after the supernatant, and collecting precipitation will precipitate and use water dissolution, crystallization, and spinning again, vacuum-drying obtains flavonoid compound.
When extracting flavonoid compound, the fluid extract deposition is 1: 3 with the mass ratio of alkaline ethanol solution; When deposition after the spinning is used water dissolution deposition and water mass ratio be 1: 1;-20 ℃ of crystallizations, 36 hours time, 3 recrystallizations; Alcohol concn is 15wt% in the said alkaline ethanol solution, and (alkali of adding or alkaline, inorganic salts are conventional, like NaOH, KOH, Na to add alkali or alkaline, inorganic salts
2CO
3, NaHCO
3, K
2CO
3, KHCO
3Or the like in one or more) to make its pH value be 10.
The present invention prepares gained isofraxidin content 91.5%, the rate of transform 60.8%, flavonoid content 95.5%, the rate of transform 82.4%.
Embodiment 6
(1) the Herba Pileae Scriptae medicinal material is ground into 4cm before adopting the hoirzontally rotating countercurrent extraction.
(2) adopt the hoirzontally rotating countercurrent extraction; Rising the membrane-concentrated vaporizer concentrates: adopting in the said hoirzontally rotating countercurrent extraction method and extracting solvent is the mixed solvent of a kind of or their any ratios in ethanol or the Virahol; Extracting solvent quality is 8 times of amounts of Herba Pileae Scriptae quality of medicinal material, and extracting temperature is 60 ℃, and extraction time is 4 times; Each extraction time is 4 hours, and the extracting solution flow is 15L/min.
(3) vacuum concentration obtains fluid extract: the solvent that extracts fluid extract is a solvent oil, and extracting solvent and fluid extract mass ratio is 8: 1, and extraction time is 4 times, collects supernatant (the fluid extract deposition after the collection supernatant is subsequent use), is concentrated into 15% of original volume; Recrystallization under the room temperature.
(4) with going up silica gel adsorption behind the dissolution of crystals; Wash-out: the crystal of recrystallization dissolves with methylene dichloride, the mass ratio of crystal and elutriant 1: 5, last silicagel column absorption; Used silica gel order number is 50 orders; The elutriant that adopts is a kind of or its arbitrary proportion mixed solvent in sherwood oil, normal hexane, solvent oil or the ETHYLE ACETATE, carries out wash-out, adopts the tlc contrast to collecting fully.
(5) low temperature crystallization obtains the high purity isofraxidin after the vacuum-drying: the crystal elutriant through behind silica gel adsorption, the wash-out is concentrated into 15% of original volume, low temperature crystallization, and Tc is 0 ℃, crystallization time is 16 hours, 3 recrystallizations.
Extraction is placed spinning after 40 hours after collecting the fluid extract deposition employing alkaline ethanol solution dissolving after the supernatant, and collecting precipitation will precipitate and use water dissolution, crystallization, and spinning again, vacuum-drying obtains flavonoid compound.
When extracting flavonoid compound, the fluid extract deposition is 1: 4 with the mass ratio of alkaline ethanol solution; When deposition after the spinning is used water dissolution deposition and water mass ratio be 1: 6;-15 ℃ of crystallizations, 30 hours time, 4 recrystallizations; Alcohol concn is 25wt% in the said alkaline ethanol solution, and (alkali of adding or alkaline, inorganic salts are conventional, like NaOH, KOH, Na to add alkali or alkaline, inorganic salts
2CO
3, NaHCO
3, K
2CO
3, KHCO
3Or the like in one or more) to make its pH value be 11.
The present invention prepares gained isofraxidin content 94.1, the rate of transform 64.8%, flavonoid content 96.7, the rate of transform 84.5.
Application implementation example 1
Isofraxidin and flavonoid compound are used to make lotion or body wash
Prescription as follows, according to mass percent: flavonoid compound 0.05-2%, isofraxidin 0.05-2%; Radix Sophorae Flavescentis extract 0.1-2%, hundred step extract 0.1-1%, lauryl sulfate 10-30%; C-30 cocoamidopropyl betaine 2-5%, pearling agent 0.5-1.5%, TC2100 silicone emulsion 0.5-3%; Essence 0.005-0.05%, all the other are pure water.Can be formulated into to have and press down the harmful bacterium that kills skin surface, lotion, the body wash of the generation of conditioning skin and prevention skin carcinoma.
Application implementation example 2
Isofraxidin and flavonoid compound are used to make health promoting beverage
Prescription as follows, according to mass percent:
Flavonoid compound 0.01-2%, isofraxidin 0.01-2%, honey 0.1-2%, vitamins C 0.1-1%, vitamins B
10.1-1%, all the other are water.It is pure and mild to can be formulated into mouthfeel, has anti-inflammatory, protects tooth, goes to lack, the health promoting beverage of effect such as beauty treatment, strengthening immunity.
Claims (6)
1. the technology of simultaneous extraction isofraxidin and flavonoid compound from a Herba Pileae Scriptae, it is characterized in that: adopt the hoirzontally rotating countercurrent extraction, the membrane-concentrated vaporizer is concentrated through rising, vacuum concentration; Obtain fluid extract, extract fluid extract 3-5 time, collect supernatant; With the supernatant concentration post crystallization; With upward silica gel adsorption behind the dissolution of crystals, low temperature crystallization behind the wash-out, Tc is-10～10 ℃; Obtain the high purity isofraxidin after the vacuum-drying; Extraction is placed spinning after 24-48 hour after collecting the fluid extract deposition employing alkaline ethanol solution dissolving after the supernatant, and collecting precipitation will precipitate and use water dissolution, crystallization, and spinning again, vacuum-drying obtains flavonoid compound; The solvent that wherein extracts fluid extract is one or more mixed solvents in chloroform, methylene dichloride, sherwood oil, normal hexane or the solvent oil; Extracting solvent and fluid extract mass ratio is 3: 1-10: 1, and extraction time is 3-5 time, collects supernatant; Be concentrated into the 5-20% of original volume, recrystallization under the room temperature.
2. according to claim 1 from Herba Pileae Scriptae the technology of simultaneous extraction isofraxidin and flavonoid compound, it is characterized in that: said Herba Pileae Scriptae medicinal material is ground into 2-5cm before adopting the hoirzontally rotating countercurrent extraction.
3. according to claim 1 from Herba Pileae Scriptae the technology of simultaneous extraction isofraxidin and flavonoid compound; It is characterized in that: adopting in the said hoirzontally rotating countercurrent extraction method and extracting solvent is one or more mixed solvents in water, methyl alcohol, ethanol or the Virahol; The extraction solvent quality is that the 3-10 of Herba Pileae Scriptae quality of medicinal material doubly measures, and extracting temperature is 30-80 ℃, and extraction time is 3-5 time; Each extraction time is 1-5 hour, and the extracting solution flow is 15L/min.
4. according to claim 1 from Herba Pileae Scriptae the technology of simultaneous extraction isofraxidin and flavonoid compound; It is characterized in that: the crystal of recrystallization is with one or more the mixed solvent dissolving in methyl alcohol, ethanol, chloroform, methylene dichloride, sherwood oil, normal hexane or the solvent oil; The mass ratio of crystal and elutriant is 1: 1-1: 8; Last silicagel column absorption, used silica gel order number is the 20-200 order, the elutriant of employing is a kind of or its arbitrary proportion mixed solvent in sherwood oil, normal hexane, solvent oil or the ETHYLE ACETATE; Carry out wash-out, adopt the tlc contrast to collecting fully.
5. according to claim 1 from Herba Pileae Scriptae the technology of simultaneous extraction isofraxidin and flavonoid compound; It is characterized in that: the 5-20% that is concentrated into original volume through the crystal elutriant behind silica gel adsorption, the wash-out; Low temperature crystallization, crystallization time are 5-24 hour, the one or many recrystallization.
6. according to claim 1 from Herba Pileae Scriptae the technology of simultaneous extraction isofraxidin and flavonoid compound, it is characterized in that: during said extraction flavonoid compound, the fluid extract deposition is 1 with the mass ratio of alkaline ethanol solution: 1-1: 5; When deposition after the spinning is used water dissolution deposition and water mass ratio be 1: 1-1: 8;-30-0 ℃ of crystallization, time 12-48 hour, one or many recrystallization; Alcohol concn is 10-30wt% in the said alkaline ethanol solution, adds alkali or alkaline, inorganic salts and makes its pH value be 8-12.
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| CN102633760B (en) * | 2012-03-20 | 2013-04-10 | 浙江维康药业有限公司 | Isofraxidin crystalline compound and glabrous sarcandra herb dispersible tablets and dropping pills containing isofraxidin crystalline compound |
| CN106967029A (en) * | 2016-01-14 | 2017-07-21 | 广东省中医院 | One kind prepares isofraxidin method from Chinese medicinal material of sarcandra glaber |
| CN107519293A (en) * | 2017-08-14 | 2017-12-29 | 海南葫芦娃药业集团股份有限公司 | A kind of benzydamine micropill and preparation method thereof |
| CN113797127B (en) * | 2021-08-31 | 2023-03-03 | 珀莱雅化妆品股份有限公司 | Plant fermentation product with black eye resisting effect and preparation method thereof |
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