CN107837299A - A kind of Scullcap total-flavonoid aglycone extracting method based on itself zymolysis technique of infrared auxiliary - Google Patents
A kind of Scullcap total-flavonoid aglycone extracting method based on itself zymolysis technique of infrared auxiliary Download PDFInfo
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- CN107837299A CN107837299A CN201610840163.XA CN201610840163A CN107837299A CN 107837299 A CN107837299 A CN 107837299A CN 201610840163 A CN201610840163 A CN 201610840163A CN 107837299 A CN107837299 A CN 107837299A
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- flavonoid aglycone
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K36/00—Medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicines
- A61K36/18—Magnoliophyta (angiosperms)
- A61K36/185—Magnoliopsida (dicotyledons)
- A61K36/53—Lamiaceae or Labiatae (Mint family), e.g. thyme, rosemary or lavender
- A61K36/539—Scutellaria (skullcap)
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- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2236/00—Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
- A61K2236/10—Preparation or pretreatment of starting material
- A61K2236/19—Preparation or pretreatment of starting material involving fermentation using yeast, bacteria or both; enzymatic treatment
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2236/00—Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
- A61K2236/30—Extraction of the material
- A61K2236/33—Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones
- A61K2236/333—Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones using mixed solvents, e.g. 70% EtOH
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Abstract
The invention belongs to analytical chemistry field, is related to a kind of Scullcap total-flavonoid aglycone extracting method based on itself zymolysis technique of infrared auxiliary.This method includes, and chooses radix scutellariae medicinal materials powder, first carries out infrared auxiliary itself enzymolysis：The cushioning liquid of water or certain pH is added as enzymolysis solution, certain temperature is controlled, carries out certain power, the infra-red radiation of certain time；Then add organic solvent and carry out infrared assisted extraction；Tested and analyzed after extract solution filtering by efficient liquid phase liquid chromatography instrument.Itself zymolysis technique of infrared auxiliary in the present invention, enzymolysis is abundant, speed is fast, efficiency high, safety and environmental protection, has the extraction for being suitable for Scullcap total-flavonoid aglycone in radix scutellariae medicinal materials, preparing for the utilization and Scullcap total-flavonoid aglycone for radix scutellariae medicinal materials is significant.
Description
Technical field
The invention belongs to analytical chemistry field, it is related to the extracting method of Scullcap total-flavonoid aglycone, and in particular to one kind is based on
The Scullcap total-flavonoid aglycone extracting method of itself zymolysis technique of infrared auxiliary.
Background technology
It is labiate radix scutellariae (Scutellaria baicalensis Georgi.) prior art discloses radix scutellariae
Dry root, see be loaded in earliest《Sheng Nong's herbal classic》.Radix scutellariae has heat-clearing and damp-drying drug, purging intense heat and detonicating, arresting bleeding and miscarriage prevention and other effects.Modern medicine
Neo-Confucianism shows that radix scutellariae has the work such as anti-bacteria and anti-virus, anti-inflammatory, anti-oxidant, antitumor, immunological regulation, antipyretic-antalgic, hepatic cholagogic
It is flavones ingredient with, its main active, including scutelloside, wogonoside, qroxylin A-grape alditol glycosides and its glycosides
First baicalein, wogonin, qroxylin A etc., scutelloside and wogonoside and its interior metabolism product are considered in the industry yellow
A kind of reed mentioned in ancient books plays the material base of drug effect.
It is mainly flavonoid glycoside composition that data, which discloses traditional enzyme guarantor's glycosides method extraction result of killing,.Drug metabolism Mechanism Study
Show, scutellaria glycosides compounds are easily combined with the glucuronic acid with larger polarity in vivo, therefore are being disappeared after being administered orally
Change road to be difficult to directly be absorbed, its major part can be excreted.Absorption of the studies have shown that baicalein at each position of alimentary canal is bright
It is aobvious to be higher than scutelloside, there is extensive absorption window, approve that scutelloside is converted into baicalein can significantly improve biological utilisation in the industry
Degree；Also there are some researches show have endogenous enzymes, under certain temperature and humidity, scutelloside can be made to change into radix scutellariae in radix scutellariae medicinal materials
Element.
Infrared assisted extraction (infrared-assisted extraction, IRAE) technology is a kind of special using infrared ray
The extractive technique of property, studies have shown that is when infrared radiation of the heating object molecule by specific frequency, i.e. the radiation of radiation source
When power spectrum is corresponding to the main absorption band Wavelength distribution of heating object, heating object molecule can be caused to produce RESONANCE ABSORPTION, accelerated
Intramolecular warm-up movement, so as to reach the purpose of heating.Practice confirmation, method safety and environmental protection, efficient energy-saving, the firing rate
It hurry up, to heat inertia small and cheap, easy to spread.At present, infrared auxiliary extraction technology has been successfully applied to some Chinese medicines
The extraction of active component, such as matrimony vine, the red sage root, grape pip, Radix picrorrhizae, frutus cnidii, the results showed that the technology can significantly improve
Extraction efficiency simultaneously significantly shortens extraction time.
The extracting method of Scullcap total-flavonoid aglycone is extracted frequently with external enzyme at present, itself enzyme water-bath is extracted etc., but these
The shortcomings that cumbersome, time-consuming or yield is low be present more in method.So far, there is not yet infrared auxiliary and radix scutellariae itself are digested
The report for the extracting method being combined.
Present situation based on prior art, present inventor intend providing a kind of efficient, quick Scullcap total-flavonoid aglycone
Extracting method, be based especially on the Scullcap total-flavonoid aglycone extracting method of itself zymolysis technique of infrared auxiliary.This method efficiently,
Quickly, simple to operate, safety and environmental protection, the extraction of Scullcap total-flavonoid aglycone can be applied to, is advantageous to the exploitation profit of radix scutellariae medicinal materials
With and Scullcap total-flavonoid aglycone preparation.
The content of the invention
The defects of it is an object of the invention to overcome prior art and deficiency, there is provided one kind is efficient, quick radix scutellariae is always yellow
The extracting method of ketoside member, especially a kind of fast, efficient, safe environmentally friendly radix scutellariae based on itself zymolysis technique of infrared auxiliary
The extracting method of total-flavonoid aglycone.
To realize the purpose, concrete technical scheme of the invention is：
A kind of Scullcap total-flavonoid aglycone extracting method based on itself zymolysis technique of infrared auxiliary：Radix scutellariae medicinal materials powder is taken,
Infrared auxiliary itself enzymolysis is first carried out, controls certain temperature, the cushioning liquid of water or certain pH is added as enzymolysis solution, enters
The certain power of row, the infra-red radiation of certain time；Then add organic solvent and carry out infrared assisted extraction；Lead to after extract solution filtering
Cross the detection and analysis of efficient liquid phase liquid chromatography instrument.
Further, the infrared assistance enzymolysis temperature is 20~60 DEG C, the Scullcap total-flavonoid aglycone in this temperature range
Recovery rate be 15.15~18.88g/100g.
Further, infrared assistance enzymolysis liquid-solid ratio (mL/g) is 5:1~60:1, Scullcap total-flavonoid aglycone within this range
Recovery rate be 14.88~19.21g/100g.
Further, infrared assistance enzymolysis liquid can be water or pH 4~6.4 cushioning liquid, and radix scutellariae is total on this condition
The recovery rate of flavone aglycone is 15.06~19.21g/100g.
Further, the infrared assistance enzymolysis infrared power is 150W~275W, and radix scutellariae is always yellow in this power bracket
The recovery rate of ketoside member is 17.86~19.21g/100g.
Further, the infrared assistance enzymolysis time is 15min~90min, the Scullcap total-flavonoid in the range of this time
The recovery rate of aglycon is 14.58~19.21g/100g.
Further, infrared extraction after the infrared assistance enzymolysis, Extraction solvent are methanol-hydrochloric acid (200:1), during extraction
Between be 20min.
In the present invention, radix scutellariae medicinal materials are taken to be extracted using this method, under conditions of different infrared assistance enzymolysis liquid,
The recovery rate of Scullcap total-flavonoid aglycone is respectively 15.15~18.88g/100g；14.88~19.21g/100g；15.06~
19.21g/100g；17.86~19.21g/100g；14.58~19.21g/100g.
The inventive method compared with the prior art, its advantage and is beneficial in that：This method is a kind of based on infrared auxiliary
Help the Scullcap total-flavonoid aglycone extracting method of itself zymolysis technique, simple to operate, abundant, the fast, efficient, safe environmental protection of enzymolysis.
Preparing for utilization and Scullcap total-flavonoid aglycone for radix scutellariae medicinal materials is significant.
Brief description of the drawings
Fig. 1 is the structural formula of baicalein, wogonin, qroxylin A.
Fig. 2 high-efficient liquid phase chromatograms,
Wherein, A：Blank solvent；B：Reference substance solution；C：Radix scutellariae extract solution
a：Baicalein；b：Wogonin；c：Qroxylin A
Fig. 3 extracting methods compare, wherein,
IRAE：Infrared assistance enzymolysis 30min；HRE-30min：Water enzyme digestion 30min；HRE-180min：Water enzyme digestion
180min。
Embodiment
The present invention is described in further detail below in conjunction with drawings and examples.
1. instrument and reagent
Instrument：The high performance liquid chromatographs of Agilent 1200, pacify the stiff matter infrared lamp of enlightening, and laboratory is made infrared auxiliary by oneself and carried
Take device.
Reagent：Baicalein reference substance (97.8%, Nat'l Pharmaceutical ＆ Biological Products Control Institute), wogonin reference substance (98%,
Wo Kai), qroxylin A reference substance (98%, Nanjing Zelang Pharmaceutical Technology Inc.)；Phosphoric acid, hydrochloric acid, citric acid, phosphoric acid hydrogen
Disodium (analyzes pure, Chemical Reagent Co., Ltd., Sinopharm Group).
Methanol (chromatographically pure, Merck companies of the U.S.), pure water are Millipore deionized waters.
2. test method and result
2.1 chromatographic condition：
Using Welch Ultimate LP-C18 (250 × 4.6mm, 5 μm) chromatographic column；It is molten with methanol (C), 0.4% phosphoric acid
Liquid (B) is mobile phase, gradient elution：C：47%~47%, B：53%~53% (0~10min)；C：47%~55%, B：
53%~45% (10~30min)；C：55%~60%, B：45%~40% (30~40min)；C：40%~40%, B：
60%~60% (40~50min)；C：40%~53%, B：60%~47% (50~55min)；C：53%~53%, B：
47%~47% (55~60min).
2.2 sample treatments and analysis
Radix scutellariae medicinal materials fine powder 0.5g is weighed, adds infrared assistance enzymolysis 30min under the conditions of pure water 20mL, 200W；It is infrared auxiliary
After helping enzymolysis to terminate, methanol-hydrochloric acid (200 is added:1) infrared extraction 20min under the conditions of 80mL, 200W, extract solution cooling, mend
Weight, is analyzed after filtering；
As a result show,
The infrared assistance enzymolysis temperature is 20~60 DEG C, and the recovery rate of Scullcap total-flavonoid aglycone is in this temperature range
15.15~18.88g/100g；
Infrared assistance enzymolysis liquid-solid ratio (mL/g) is 5:1~60:1, the recovery rate of Scullcap total-flavonoid aglycone within this range
For 14.88~19.21g/100g；
Infrared assistance enzymolysis liquid can be water or pH 4~6.4 cushioning liquid, on this condition Scullcap total-flavonoid aglycone
Recovery rate be 15.06~19.21g/100g；
The infrared assistance enzymolysis infrared power is 150W~275W, and Scullcap total-flavonoid aglycone carries in this power bracket
It is 17.86~19.21g/100g to take rate；
The infrared assistance enzymolysis time is 15min~90min, the extraction of Scullcap total-flavonoid aglycone in the range of this time
Rate is 14.58~19.21g/100g.
Further, infrared extraction after the infrared assistance enzymolysis, Extraction solvent are methanol-hydrochloric acid (200:1), during extraction
Between be 20min '
Analysis result confirms that this method is simple to operate, enzymolysis is abundant, fast, efficient, safe environmental protection；Have and be suitable for radix scutellariae medicine
The utilization of material and the preparation of Scullcap total-flavonoid aglycone.
Claims (7)
- A kind of 1. Scullcap total-flavonoid aglycone extracting method based on itself zymolysis technique of infrared auxiliary, it is characterised in that it includes, Radix scutellariae medicinal materials powder is taken, infrared auxiliary itself enzymolysis is first carried out, controls certain temperature, adds water or the cushioning liquid of certain pH As enzymolysis solution, certain power, the infra-red radiation of certain time are carried out；Then the infrared auxiliary of organic solvent progress is added to carry Take；Tested and analyzed after extract solution filtering by efficient liquid phase liquid chromatography instrument.
- 2. extracting method according to claim 1, it is characterised in that：The infrared assistance enzymolysis temperature is 20~60 DEG C, The recovery rate of Scullcap total-flavonoid aglycone is 15.15~18.88g/100g in this temperature range.
- 3. according to the extracting method described in claims 1, it is characterised in that：The infrared assistance enzymolysis liquid-solid ratio mL/g is 5: 1~60:1, the recovery rate of Scullcap total-flavonoid aglycone is 14.88~19.21g/100g within this range.
- 4. extracting method according to claim 1, it is characterised in that：The infrared assistance enzymolysis liquid be water or pH 4~ 6.4 cushioning liquid, the recovery rate of Scullcap total-flavonoid aglycone is 15.06~19.21g/100g in the range of this pH.
- 5. extracting method according to claim 1, it is characterised in that：The infrared assistance enzymolysis infrared power be 150W~ 275W, the recovery rate of Scullcap total-flavonoid aglycone is 17.86~19.21g/100g in this power bracket.
- 6. extracting method according to claim 1, it is characterised in that：The infrared assistance enzymolysis time be 15min~ 90min, the recovery rate of Scullcap total-flavonoid aglycone is 14.58~19.21g/100g in the range of this time.
- 7. extracting method according to claim 1, it is characterised in that：Infrared extraction after the infrared assistance enzymolysis, extraction Solvent is methanol-hydrochloric acid 200:1, extraction time 20min.
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Cited By (3)
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| CN113229306A (en) * | 2021-04-29 | 2021-08-10 | 焙之道食品(福建)有限公司 | Preparation method of compound premixed powder |
| CN115397450A (en) * | 2020-03-04 | 2022-11-25 | 爱西美公司 | Method for producing scutellaria root hydrolysate, hydrolysate obtained by the method and application of the hydrolysate in cosmetics and dermatology grade cosmetics |
| CN115397450B (en) * | 2020-03-04 | 2024-05-24 | 爱西美公司 | Method for producing a hydrolysate of radix Scutellariae, hydrolysate obtained by the method and its application in cosmetics and dermatological cosmetics |
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| CN113229306A (en) * | 2021-04-29 | 2021-08-10 | 焙之道食品(福建)有限公司 | Preparation method of compound premixed powder |
| CN113229306B (en) * | 2021-04-29 | 2024-02-27 | 焙之道食品(福建)有限公司 | Preparation method of compound premixed flour |
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Application publication date: 20180327 |