CN106038828A - Callicarpa nudiflora extract containing rich verbascoside and preparation method of callicarpa nudiflora extract - Google Patents
Callicarpa nudiflora extract containing rich verbascoside and preparation method of callicarpa nudiflora extract Download PDFInfo
- Publication number
- CN106038828A CN106038828A CN201610401513.2A CN201610401513A CN106038828A CN 106038828 A CN106038828 A CN 106038828A CN 201610401513 A CN201610401513 A CN 201610401513A CN 106038828 A CN106038828 A CN 106038828A
- Authority
- CN
- China
- Prior art keywords
- callicarpa nudiflora
- verbascoside
- nudiflora extract
- preparation
- extract
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Classifications
-
- 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)
- A61K36/85—Verbenaceae (Verbena family)
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K31/00—Medicinal preparations containing organic active ingredients
- A61K31/70—Carbohydrates; Sugars; Derivatives thereof
- A61K31/7028—Compounds having saccharide radicals attached to non-saccharide compounds by glycosidic linkages
- A61K31/7034—Compounds having saccharide radicals attached to non-saccharide compounds by glycosidic linkages attached to a carbocyclic compound, e.g. phloridzin
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07H—SUGARS; DERIVATIVES THEREOF; NUCLEOSIDES; NUCLEOTIDES; NUCLEIC ACIDS
- C07H1/00—Processes for the preparation of sugar derivatives
- C07H1/06—Separation; Purification
- C07H1/08—Separation; Purification from natural products
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07H—SUGARS; DERIVATIVES THEREOF; NUCLEOSIDES; NUCLEOTIDES; NUCLEIC ACIDS
- C07H15/00—Compounds containing hydrocarbon or substituted hydrocarbon radicals directly attached to hetero atoms of saccharide radicals
- C07H15/18—Acyclic radicals, substituted by carbocyclic rings
-
- 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
- A61K2236/10—Preparation or pretreatment of starting material
- A61K2236/19—Preparation or pretreatment of starting material involving fermentation using yeast, bacteria or both; enzymatic treatment
-
- 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
- A61K2236/331—Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones using water, e.g. cold water, infusion, tea, steam distillation, decoction
-
- 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
- A61K2236/39—Complex extraction schemes, e.g. fractionation or repeated extraction steps
-
- 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
- A61K2236/50—Methods involving additional extraction steps
- A61K2236/51—Concentration or drying of the extract, e.g. Lyophilisation, freeze-drying or spray-drying
-
- 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
- A61K2236/50—Methods involving additional extraction steps
- A61K2236/55—Liquid-liquid separation; Phase separation
Landscapes
- Health & Medical Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Natural Medicines & Medicinal Plants (AREA)
- Organic Chemistry (AREA)
- General Health & Medical Sciences (AREA)
- Molecular Biology (AREA)
- Engineering & Computer Science (AREA)
- Biotechnology (AREA)
- Genetics & Genomics (AREA)
- Biochemistry (AREA)
- Medicinal Chemistry (AREA)
- Pharmacology & Pharmacy (AREA)
- Epidemiology (AREA)
- Animal Behavior & Ethology (AREA)
- Veterinary Medicine (AREA)
- Public Health (AREA)
- Alternative & Traditional Medicine (AREA)
- Mycology (AREA)
- Microbiology (AREA)
- Medical Informatics (AREA)
- Botany (AREA)
- Medicines Containing Plant Substances (AREA)
Abstract
The invention discloses a callicarpa nudiflora extract containing rich verbascoside and a preparation method of the callicarpa nudiflora extract and relates to the field of preparation of traditional Chinese medicines. The content of verbascoside in the callicarpa nudiflora extract containing the rich verbascoside is 10%-20%. The preparation method sequentially comprises steps as follows: a callicarpa nudiflora medicinal material and cellulose are added to water and heated for enzymolysis, the medicinal material after enzymolysis and enzymatic hydrolysate are subjected to ultrasonic filtration, herb residues are subjected to ultrasonic rehydration, filtrate is combined after filtration and concentrated, and a concentrated solution is obtained; the concentrated solution is adsorbed by macroreticular resin, and an eluent is collected; the eluent is concentrated to form thick paste, the thick paste is dried and crushed, and the callicarpa nudiflora extract is obtained. Effective ingredients are more completely dissolved out, and the yield of verbascoside and other effective ingredients is improved; the content of verbascoside in the extract is increased, and follow-up application of preparations is facilitated.
Description
Technical field
The present invention relates to field of traditional Chinese medicine pharmacy, be specifically related to a kind of Callicarpa nudiflora extract rich in verbascoside and
Preparation method.
Background technology
The main chemical compositions of Callicarpa nudiflora is the compositions such as flavonoid, terpenoid, phenolic acids, phenethyl alcohol glycosides, polysaccharide.Grind
Studying carefully display, in Callicarpa nudiflora, flavonoid, phenolic acids, phenylethanoid glycoside all have certain anti-inflammation hemostasia effect, wherein hair stamen
Flower glucosides has significant antibacterial and anti-inflammation functions.When antibacterial, the antiinflammatory that are Study of indices Callicarpa nudiflora extractum with verbascoside
During with the pharmacological action stopped blooding, test result indicate that, along with the rising of verbascoside content, the antibacterial work of Callicarpa nudiflora extractum
All can strengthen with anastalsis.
Some researchs are had been carried out at present in terms of the assay and preparation technology of Callicarpa nudiflora.Patent
CN201010289134.1 discloses the assay method of verbascoside content in Callicarpa nudiflora preparation, can effectively detect naked
Verbascoside content in flower Folium Callicarpae Formosanae extract and preparation.Patent CN201010508474.9 discloses a kind of Callicarpa nudiflora and carries
Take thing and its production and use.By the method using ultrasonic extractor to extract, total effective ingredient is the most complete and phase
Higher to content；And without heating, save the energy, extraction ratio is high.
But, Chinese medicine contains plurality of active ingredients, and with protein, cellulose, chlorophyll, natural gum, tannin, starch, plant
The non-required compositions such as fibres mix.On the one hand these compositions affect the leaching of active component in plant cell, the most also
Affect the clarity of liquid preparation of Chinese medicine.When traditional extracting method extracts, temperature is high, and extraction ratio is low, wastes solvent, cost
Height, dangerous.
Summary of the invention
It is an object of the invention to provide a kind of Callicarpa nudiflora extract rich in verbascoside.
It is a further object of the present invention to provide the preparation method of a kind of Callicarpa nudiflora extract rich in verbascoside.
The present invention is to be realized by following technical scheme.
Of the present invention is 10%-20% rich in verbascoside content in the Callicarpa nudiflora extract of verbascoside.
The preparation method of the Callicarpa nudiflora extract rich in verbascoside of the present invention, includes following successively
Step:
(1) cellulase of Callicarpa nudiflora medical material and medical material weight 0.01%～0.1% is joined medical material weight 4～8 times amount
In water, heating enzymolysis, hydrolysis temperature is 30～55 DEG C, and enzymolysis time is 30～90 minutes；
(2) by the medical material after step (1) enzymolysis and enzymolysis solution supersound extraction 20～40 minutes, filtering, medicinal residues add 4～8 times
The water of amount, supersound extraction 10～20 minutes, filter, merge twice filtrate, be concentrated to give concentrated solution；
(3) by step (2) gained concentrated solution through absorption with macroporous adsorbent resin, successively with water, 50% ethanol elution, each eluent is used
Amount is respectively 2～8 times amount column volumes；Collect 50% ethanol elution；
(4) by step (3) gained 50% ethanol elution, after reclaiming ethanol, concentrating under reduced pressure becomes thick paste, and thick paste is done through microwave vacuum again
The modes such as dry or microwave drying, vacuum drying, lyophilization, hot air drying, spray drying are dried, and pulverize, obtain Callicarpa nudiflora and carry
Taking thing, the water content of Callicarpa nudiflora extract is less than 5%, and Callicarpa nudiflora extract yield is 2%～4%.
The invention has the beneficial effects as follows: by cellulase degradation and ultrasonic extraction, crude drug cell wall is ruptured, pass through enzyme
Cell wall is more leniently loosened, ruptures by reaction, reduces resistance to mass tranfer, and the release accelerating effective ingredient is extracted.Effective ingredient
Dissolution is the most complete, improves the yield of the effective ingredient such as verbascoside；Simultaneously by purification with macroreticular resin, to hair stamen
The effective ingredient such as flower glucosides are enriched with, and improve the content of verbascoside in extract, follow-up formulation application.
Compared with the preparation method of Callicarpa nudiflora extract in patent CN201010508474.9, advantages of the present invention exists
In: by the way of cellulase degradation, add the dissolution of the effective ingredient such as verbascoside；Pure by macroporous adsorbent resin
Change, improve the content of the effective ingredient such as verbascoside in extract.
Detailed description of the invention
Below by embodiment, the present invention is described further.
Enzymolysis 90 minutes at embodiment 1: take Callicarpa nudiflora medical material 1kg, addition 0.1g cellulase, add 4L water, with 55 DEG C.
Medical material and enzymolysis solution after enzymolysis extract 40 minutes under ultrasonic frequency 40kHz, filter；Medicinal residues add 4L water, ultrasonic
Extract 20 minutes under wave frequency 40kHz, filter, merge twice filtrate, be concentrated to give concentrated solution 1.5L.
Concentrated solution is after the D101 absorption with macroporous adsorbent resin of column volume 1L, and with the water elution of 4L, water elution liquid discards；Again
With the 50% ethanol solution eluting of 6L, collect 50% ethanol elution.After 50% ethanol elution reclaims ethanol, at 0.85MPa, 60
DEG C it is concentrated in vacuo, obtains thick paste 200ml.Thick paste is again through 0.85MPa, and 70 DEG C are dried under vacuum to water content less than 5%, pulverizes, obtains naked
Flower Folium Callicarpae Formosanae extract 27g, in extract, verbascoside content is 16.4%.
Enzymolysis 30min at embodiment 2: take Callicarpa nudiflora medical material 1kg, addition 1g cellulase, add 8L water, with 35 DEG C.Enzyme
Medical material and enzymolysis solution after solution extract 20 minutes under ultrasonic frequency 40kHz, filter；Medicinal residues add 8L water, at ultrasound wave
Extract 10 minutes under frequency 40kHz, filter, merge twice filtrate, be concentrated to give concentrated solution 1.5L.
Concentrated solution is after the D101 absorption with macroporous adsorbent resin of column volume 1L, and with the water elution of 6L, water elution liquid discards；Again
With the 50% ethanol solution eluting of 8L, collect 50% ethanol elution.After 50% ethanol elution reclaims ethanol, at 0.85MPa, 60
DEG C it is concentrated in vacuo, obtains thick paste 150ml.Thick paste again through hot air drying to water content less than 5%, obtain Callicarpa nudiflora extract 38g,
In extract, verbascoside content is 11.1%.
Enzymolysis 60min at embodiment 3: take Callicarpa nudiflora medical material 1kg, addition 0.5g cellulase, add 6L water, with 45 DEG C.
Medical material and enzymolysis solution after enzymolysis extract 30 minutes under ultrasonic frequency 40kHz, filter；Medicinal residues add 6L water, ultrasonic
Extract 15 minutes under wave frequency 40kHz, filter, merge twice filtrate, be concentrated to give concentrated solution 1.5L.
Concentrated solution is after the D101 absorption with macroporous adsorbent resin of column volume 1L, and with the water elution of 6L, water elution liquid discards；Again
With the 50% ethanol solution eluting of 6L, collect 50% ethanol elution.After 50% ethanol elution reclaims ethanol, at 0.85MPa, 60
DEG C it is concentrated in vacuo, obtains thick paste 200ml.Thick paste-20 DEG C of vacuum lyophilizations of warp again, to water content less than 5%, obtain Callicarpa nudiflora and carry
Taking thing 32g, in extract, verbascoside content is 15.1%.
Claims (4)
1. the Callicarpa nudiflora extract rich in verbascoside, it is characterised in that: in described extract, verbascoside contains
Amount is 10%-20%.
2. the preparation method of a kind of Callicarpa nudiflora extract rich in verbascoside described in claim 1, it is characterised in that
Include following step successively:
The cellulase of Callicarpa nudiflora medical material and medical material weight 0.01%～0.1% is joined the water of medical material weight 4～8 times amount
In, heat enzymolysis；
By the medical material after step (1) enzymolysis and enzymolysis solution supersound extraction 20～40 minutes, filtering, medicinal residues add 4～8 times amount
Water, supersound extraction 10～20 minutes, filter, merge twice filtrate, be concentrated to give concentrated solution；
By step (2) gained concentrated solution through absorption with macroporous adsorbent resin, successively with water, 50% ethanol elution, each eluent consumption divides
It is not 2～8 times amount column volumes；Collect 50% ethanol elution；
By step (3) gained 50% ethanol elution, after reclaiming ethanol, concentrating under reduced pressure becomes thick paste, thick paste drying again, pulverizes,
Callicarpa nudiflora extract, the water content of Callicarpa nudiflora extract is less than 5%, and Callicarpa nudiflora extract yield is 2%～4%.
The preparation method of a kind of Callicarpa nudiflora extract rich in verbascoside the most according to claim 2, its feature
Being: in described step (1), hydrolysis temperature is 30～55 DEG C, enzymolysis time is 30～90 minutes.
The preparation method of a kind of Callicarpa nudiflora extract rich in verbascoside the most according to claim 2, its feature
It is: in described step (1), drying mode is microwave vacuum drying or microwave drying, vacuum drying, lyophilization, hot air drying
Any one in dry, spray dried form.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610401513.2A CN106038828A (en) | 2016-06-10 | 2016-06-10 | Callicarpa nudiflora extract containing rich verbascoside and preparation method of callicarpa nudiflora extract |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610401513.2A CN106038828A (en) | 2016-06-10 | 2016-06-10 | Callicarpa nudiflora extract containing rich verbascoside and preparation method of callicarpa nudiflora extract |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN106038828A true CN106038828A (en) | 2016-10-26 |
Family
ID=57170575
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201610401513.2A Pending CN106038828A (en) | 2016-06-10 | 2016-06-10 | Callicarpa nudiflora extract containing rich verbascoside and preparation method of callicarpa nudiflora extract |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN106038828A (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107973861A (en) * | 2017-11-24 | 2018-05-01 | 海南制药厂有限公司 | A kind of method for preparing polysaccharide from callicarpa nudiflora middle extraction |
| CN109363994A (en) * | 2018-12-07 | 2019-02-22 | 安阳工学院 | A kind of rosemary tears facial mask and preparation method thereof |
| CN109776631A (en) * | 2019-01-30 | 2019-05-21 | 中国人民解放军联勤保障部队第九二八医院 | A kind of preparation method of acteoside |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101629198A (en) * | 2009-08-04 | 2010-01-20 | 中山大学 | Method for producing monomeric compounds of acteoside |
| CN102204998A (en) * | 2010-11-30 | 2011-10-05 | 江西普正制药有限公司 | Method for measuring content of verbascoside in callicarpa nudiflora preparation |
| CN103816296A (en) * | 2012-11-19 | 2014-05-28 | 苏州润新生物科技有限公司 | Callicarpa bodinieri total glycosides extract as well as preparation method and application thereof |
| CN104530147A (en) * | 2014-11-27 | 2015-04-22 | 普正药业股份有限公司 | Method for preparing verbascoside standard product from callicarpa nudiflora leaf |
| CN104644882A (en) * | 2015-01-05 | 2015-05-27 | 海南医学院 | Callicarpa nudiflora extract containing phenylethanoid glycoside and preparation method thereof |
-
2016
- 2016-06-10 CN CN201610401513.2A patent/CN106038828A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101629198A (en) * | 2009-08-04 | 2010-01-20 | 中山大学 | Method for producing monomeric compounds of acteoside |
| CN102204998A (en) * | 2010-11-30 | 2011-10-05 | 江西普正制药有限公司 | Method for measuring content of verbascoside in callicarpa nudiflora preparation |
| CN103816296A (en) * | 2012-11-19 | 2014-05-28 | 苏州润新生物科技有限公司 | Callicarpa bodinieri total glycosides extract as well as preparation method and application thereof |
| CN104530147A (en) * | 2014-11-27 | 2015-04-22 | 普正药业股份有限公司 | Method for preparing verbascoside standard product from callicarpa nudiflora leaf |
| CN104644882A (en) * | 2015-01-05 | 2015-05-27 | 海南医学院 | Callicarpa nudiflora extract containing phenylethanoid glycoside and preparation method thereof |
Non-Patent Citations (1)
| Title |
|---|
| 高建德等: "纤维素酶提取肉苁蓉中苯乙醇苷的工艺研究", 《中药材》 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107973861A (en) * | 2017-11-24 | 2018-05-01 | 海南制药厂有限公司 | A kind of method for preparing polysaccharide from callicarpa nudiflora middle extraction |
| CN109363994A (en) * | 2018-12-07 | 2019-02-22 | 安阳工学院 | A kind of rosemary tears facial mask and preparation method thereof |
| CN109776631A (en) * | 2019-01-30 | 2019-05-21 | 中国人民解放军联勤保障部队第九二八医院 | A kind of preparation method of acteoside |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| Chen et al. | Optimization of ultrasonic extraction process of polysaccharides from Ornithogalum Caudatum Ait and evaluation of its biological activities | |
| CN101396384B (en) | Asiatic centella extract and preparation methode thereof | |
| CN107595893A (en) | A kind of enzyme treated prepared slices of Chinese crude drugs and preparation method thereof | |
| CN104906153A (en) | Technological method for efficiently extracting ginkgo flavone | |
| CN101585885A (en) | Method for preparing polygonatum odoratum polysaccharide | |
| CN102127140A (en) | Method for combinedly extracting Morroniside, dogwood polysaccharide and ursolic acid from dogwood | |
| CN103467617A (en) | Method for continuous counter-current ultrasonic extraction of high-purity astragalus polysaccharide | |
| CN105816518A (en) | Walnut green seedcase phenol natural antioxidant and preparing method and application thereof | |
| CN101524458B (en) | Extract of smilax glabra saponins and flavonoid and preparation method thereof | |
| CN103191196A (en) | Integrated ultrasonic cyclic extracting and separating technology for cistanche functional ingredient | |
| CN106038828A (en) | Callicarpa nudiflora extract containing rich verbascoside and preparation method of callicarpa nudiflora extract | |
| CN101284120A (en) | Process for preparing Pingxiao preparation | |
| CN105504079A (en) | Process for producing astragalus polysaccharide by using ultrasonic technology | |
| Wei et al. | Dienzyme-assisted salting-out extraction of flavonoids from the seeds of Cuscuta chinensis Lam. | |
| CN101538296B (en) | Active ingredients of camptosorus sibiricus, and extraction method and use of same | |
| CN102233013A (en) | Preparation method for total saponins of pulsatilla chinensis | |
| CN104940280A (en) | Method for extracting total flavones from radix puerariae employing enzyme preparation | |
| CN101955479A (en) | Method for extracting orientin from bamboo leaf | |
| CN109170885A (en) | A method of extracting ginseng effective component | |
| CN108358822A (en) | A method of continuously extracting a variety of active ingredients from matrimony vine cull fruit | |
| CN102617696B (en) | Preparation method of asiaticoside | |
| CN102091107B (en) | Method for extracting total triterpene of centella asiatica by enzymic process | |
| CN108126000B (en) | Method for extracting and preparing panax notoginseng saponins from fresh panax notoginseng | |
| CN103570798B (en) | Method for producing perilla nankinensis sterol by perilla nankinensis cakes | |
| CN108743657A (en) | The preparation method of methods of glycosides in a kind of mussot swertia herb |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20161026 |
|
| WD01 | Invention patent application deemed withdrawn after publication |