CN102225091A - Method for preparing barbat skullcap total polyphenol - Google Patents
Method for preparing barbat skullcap total polyphenol Download PDFInfo
- Publication number
- CN102225091A CN102225091A CN2011101178991A CN201110117899A CN102225091A CN 102225091 A CN102225091 A CN 102225091A CN 2011101178991 A CN2011101178991 A CN 2011101178991A CN 201110117899 A CN201110117899 A CN 201110117899A CN 102225091 A CN102225091 A CN 102225091A
- Authority
- CN
- China
- Prior art keywords
- herba scutellariae
- scutellariae barbatae
- alcohol
- total polyphenols
- preparation
- 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
Abstract
The invention provides a method for preparing barbat skullcap total polyphenol, which comprises the following steps: crushing whole plant of barbat skullcap, well mixing distilled water containing with cellulose, wherein the constant temperature is 30 DEG C to 50 DEG C, performing an enzymatic hydrolysis for 1 - 3 hours, killing enzyme with high temperature after finishing the enzymatic hydrolysis, extracting by using a water constant temperature continuous countercurrent method, collecting water extraction and residue, backflow extracting residue by using alcohol, merging the water extraction and alcohol extract, precipitating by adding a plurality of alcohol, filtering and removing impurity, concentrating and drying to obtain barbat skullcap total polyphenol. The method has the advantages of simple operation, complete extraction, and is suitable for scale industrial production.
Description
Technical field:
The present invention relates to the Separation of Natural Products field, particularly relate to a kind of preparation method from the Herba Scutellariae Barbatae total polyphenols.
Background technology:
Herba Scutellariae Barbatae (Scutellaria barbata D.Don), according to " Chinese pharmacopoeia is recorded, and certified products is a Labiatae Scutellaria plant, call into narrow leaf Herba Scutellariae indicae, and head grass, toothbrush careless, with dry herb, with all herbal medicine.Herba Scutellariae Barbatae distributes very extensive in China, except northeast severe cold areas and area, sandy wasteland, northwest, almost all there is distribution the each province, mostly is wild.Its head sees Jiang Yi " medicine mirror pick up any lost article from the road tax ": " Herba Scutellariae Barbatae is separated the Herba mesonae chinensis of snakebite ".The Herba Scutellariae Barbatae herb contains flavonoid, Diterpenes, polysaccharide, alkaloid, volatilization wet goods various active composition.
The Herba Scutellariae Barbatae function cures mainly and is heat clearing away, detoxifcation, dissipating blood stasis, hemostasis, analgesic therapy.Control haematemesis, epistaxis, stranguria with blood, bloody dysentery, jaundice is had sore throat, lung abscess, furuncle, scrofula, sore, cancerous protuberance, traumatic injury knife injury, venom etc.Modern pharmacological research shows that Herba Scutellariae Barbatae also has the antineoplastic activity.Dong Huan is joyous, and the water that waits the antineoplastic component that studies show that Herba Scutellariae Barbatae mainly to be present in it is carried or the alcohol extraction part; The antioxidant activity that also draws Herba Scutellariae Barbatae simultaneously exists with Herba Scutellariae Barbatae total phenols and total flavones component and concerns.Chinese scholars is more to its flavones ingredient extraction separation research report in recent years, and to the rarely seen report of the research of polyphenols in the Herba Scutellariae Barbatae.Polyphenols has the natural product of unique physiology and pharmacologically active as a class, all has good effect at aspects such as antimutagenic, antitumor, antiviral, antimicrobial, defying age, antioxidation.
Prior art mainly rests on the extraction separation of its flavonoid substance Herba Scutellariae Barbatae research, relates to less to the research of Herba Scutellariae Barbatae total polyphenols." Herba Scutellariae Barbatae total polyphenols assay and the ultrasonic extraction process research " that Wang Tieshan etc. deliver, the disclosed optimum extraction process of the document is 65% ethanol ultrasonic extraction 45min of 35 times of amounts, the quantity of solvent that the document adopts is bigger, and only makes crude extract, does not obtain Herba Scutellariae Barbatae polyphenol product.
Summary of the invention:
The preparation method that the purpose of this invention is to provide a kind of Herba Scutellariae Barbatae total polyphenols.
The objective of the invention is to realize by following proposal:
A kind of preparation method of Herba Scutellariae Barbatae total polyphenols is characterized in that: the Herba Scutellariae Barbatae herb is pulverized, with the distilled water mixing that is mixed with cellulase, 30～50 ℃ of constant temperature, enzymolysis 1～3h, enzymolysis finish back high temperature enzyme denaturing, adopt the lixiviate of 6～10 times of water termostat continuous countercurrent techniques again, collect water extract and residue; Residue adopts 6～10 times 30～65% alcohol reflux again, gets alcohol extract; Above-mentioned water extract and alcohol extract are merged, add alcohol precipitation, remove impurity, concentrate drying gets the Herba Scutellariae Barbatae total polyphenols.
Described cellulase consumption is 1～6% of a material.
Described high temperature enzyme denaturing step is a heated and boiled, protects the 15min that boils.
Described Continuous Countercurrent Extraction method is divided into 4～8 unit, and thermostatic control is at 40～70 ℃, and extraction time is 2～5h.
Described alcohol reflux number of times is 1～3 time, and extraction time is 0.5～3h, and the control temperature is 60～80 ℃.
Described alcohol precipitation reaches 70% for adding ethanol to determining alcohol.
Described drying means is a kind of in lyophilization, spray drying or the low-temperature vacuum drying.
Advantage of the present invention is: this method is simple to operate, extraction is complete; Solvent is saved in the continuous countercurrent technique lixiviate, the enzymatic isolation method reaction temperature and, the yield height; Solvent for use toxicity is little, recyclable repeated use, and environmental pollution is little, is fit to industrial scale production.
The specific embodiment:
Further specify the present invention by the following examples, but not as limitation of the present invention.
Embodiment 1
Getting the Herba Scutellariae Barbatae herb pulverizes, get 1kg, adding 5L is mixed with the distilled water mixing of 10g cellulase, 50 ℃ of constant temperature, stir enzymolysis 1h, enzymolysis finishes post-heating and protects the 15min enzyme denaturing that boils, and adds 6L70 ℃ of water termostat dynamic countercurrent lixiviate 5h again, extraction is divided into 4 unit to be carried out, and centrifugalize gets water extract and residue; Residue adds 60 ℃ of reflux, extract, 3h of 30% ethanol constant temperature of 6L again, gets alcohol extract; Above-mentioned water extract and alcohol extract are merged, add ethanol to determining alcohol and reach 70%, remove by filter impurity such as protein, polysaccharide, the dry Herba Scutellariae Barbatae total polyphenols 10.3g that gets of filtrate concentrated spray, content reaches more than 50%.
Embodiment 2
Getting the Herba Scutellariae Barbatae herb pulverizes, get 1kg, adding 6L is mixed with the distilled water mixing of 60g cellulase, 30 ℃ of constant temperature, stir enzymolysis 3h, enzymolysis finishes post-heating and protects the 15min enzyme denaturing that boils, and adds 10L40 ℃ of water termostat dynamic countercurrent lixiviate 2h again, extraction is divided into 8 unit to be carried out, and centrifugalize gets water extract and residue; Residue adds 80 ℃ of reflux, extract, of 65% ethanol constant temperature 3 times of 10L again, each 0.5h, merge alcohol extract; Above-mentioned water extract and alcohol extract are merged, add ethanol to determining alcohol and reach 70%, remove by filter impurity such as protein, polysaccharide, the dry Herba Scutellariae Barbatae total polyphenols 13.1g that gets of filtrate concentrated frozen, content reaches more than 50%.
Embodiment 3
Getting the Herba Scutellariae Barbatae herb pulverizes, get 5kg, adding 20L is mixed with the distilled water mixing of 100g cellulase, 45 ℃ of constant temperature, stir enzymolysis 1.5h, enzymolysis finishes post-heating and protects the 15min enzyme denaturing that boils, and adds 40L50 ℃ of water termostat dynamic countercurrent lixiviate 3h again, extraction is divided into 5 unit to be carried out, and centrifugalize gets water extract and residue; Residue adds 65 ℃ of reflux, extract, of 40% ethanol constant temperature 2 times of 30L again, each 1h, alcohol extract; Above-mentioned lixiviating solution, enzymolysis solution and alcohol extract are merged, add ethanol to determining alcohol and reach 70%, remove by filter impurity such as protein, polysaccharide, filtrate concentrating low-temperature vacuum drying gets Herba Scutellariae Barbatae total polyphenols 49.8g, and content reaches more than 50%.
Embodiment 4
Getting the Herba Scutellariae Barbatae herb pulverizes, get 10kg, adding 50L is mixed with the distilled water mixing of 220g cellulase, 35 ℃ of constant temperature, stir enzymolysis 2h, enzymolysis finishes post-heating and protects the 15min enzyme denaturing that boils, and adds 100L55 ℃ of water termostat dynamic countercurrent lixiviate 3.5h again, extraction is divided into 6 unit to be carried out, and centrifugalize gets water extract and residue; Residue adds 70 ℃ of reflux, extract, 2h of 45% ethanol constant temperature of 70L again, gets alcohol extract; Above-mentioned lixiviating solution, enzymolysis solution and alcohol extract are merged, add ethanol to determining alcohol and reach 70%, remove by filter impurity such as protein, polysaccharide, the dry Herba Scutellariae Barbatae total polyphenols 94.9g that gets of filtrate concentrated spray, content reaches more than 50%.
Embodiment 5
Getting the Herba Scutellariae Barbatae herb pulverizes, get 10kg, adding 60L is mixed with the distilled water mixing of 500g cellulase, 45 ℃ of constant temperature, stir enzymolysis 2.5h, enzymolysis finishes post-heating and protects the 15min enzyme denaturing that boils, and adds 80L65 ℃ of water termostat dynamic countercurrent lixiviate 4h again, extraction is divided into 7 unit to be carried out, and centrifugalize gets water extract and residue; Residue adds 75 ℃ of reflux, extract, 2.5h of 50% ethanol constant temperature of 80L again, gets alcohol extract; Above-mentioned lixiviating solution, enzymolysis solution and alcohol extract are merged, add ethanol to determining alcohol and reach 70%, remove by filter impurity such as protein, polysaccharide, the dry Herba Scutellariae Barbatae total polyphenols 105.7g that gets of filtrate concentrated spray, content reaches more than 50%.
Claims (5)
1. the preparation method of a Herba Scutellariae Barbatae total polyphenols is characterized in that: the Herba Scutellariae Barbatae herb is pulverized, with the distilled water mixing that is mixed with cellulase, 30～50 ℃ of constant temperature, enzymolysis 1～3h, enzymolysis finish back high temperature enzyme denaturing, adopt the lixiviate of 6～10 times of water termostat continuous countercurrent techniques again, collect water extract and residue; Residue adopts 6～10 times 30～65% alcohol reflux again, gets alcohol extract; Above-mentioned water extract and alcohol extract are merged, add alcohol precipitation, remove impurity, concentrate drying gets the Herba Scutellariae Barbatae total polyphenols.
2. the preparation method of a kind of Herba Scutellariae Barbatae total polyphenols as claimed in claim 1 is characterized in that described cellulase consumption is 1～6% of a medical material amount.
3. the preparation method of a kind of Herba Scutellariae Barbatae total polyphenols as claimed in claim 1 is characterized in that described Continuous Countercurrent Extraction method is divided into 4～8 unit, and thermostatic control is at 40～70 ℃, and extraction time is 2～5h.
4. the preparation method of a kind of Herba Scutellariae Barbatae total polyphenols as claimed in claim 1 is characterized in that described alcohol reflux number of times is 1～3 time, and extraction time is 0.5～3h, and the control temperature is 60～80 ℃.
5. the preparation method of a kind of Herba Scutellariae Barbatae total polyphenols as claimed in claim 1 is characterized in that described drying means is a kind of in lyophilization, spray drying or the low-temperature vacuum drying.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2011101178991A CN102225091A (en) | 2011-05-06 | 2011-05-06 | Method for preparing barbat skullcap total polyphenol |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2011101178991A CN102225091A (en) | 2011-05-06 | 2011-05-06 | Method for preparing barbat skullcap total polyphenol |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN102225091A true CN102225091A (en) | 2011-10-26 |
Family
ID=44806120
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN2011101178991A Pending CN102225091A (en) | 2011-05-06 | 2011-05-06 | Method for preparing barbat skullcap total polyphenol |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN102225091A (en) |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102631380A (en) * | 2012-04-18 | 2012-08-15 | 东北林业大学 | Method and device for extracting polyphenol substance from Korean pine shells |
| CN102631381A (en) * | 2012-04-18 | 2012-08-15 | 东北林业大学 | Method for extracting polyphenol substance from Korean pine barks |
| CN106902540A (en) * | 2017-04-21 | 2017-06-30 | 浩宇康宁健康科技（湖北）有限公司 | The holographic biochemistry high-valued extraction separation method of physics coupled system of Chinese medicine and Magnolia cortex P.E |
| CN107372966A (en) * | 2017-08-21 | 2017-11-24 | 紫云自治县红花茶业种植有限公司 | A kind of balloonflower root jasmine tea and preparation method thereof |
| CN115067534A (en) * | 2022-07-11 | 2022-09-20 | 湖北中烟工业有限责任公司 | Preparation method of vine tea extract for cigarettes |
-
2011
- 2011-05-06 CN CN2011101178991A patent/CN102225091A/en active Pending
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102631380A (en) * | 2012-04-18 | 2012-08-15 | 东北林业大学 | Method and device for extracting polyphenol substance from Korean pine shells |
| CN102631381A (en) * | 2012-04-18 | 2012-08-15 | 东北林业大学 | Method for extracting polyphenol substance from Korean pine barks |
| CN106902540A (en) * | 2017-04-21 | 2017-06-30 | 浩宇康宁健康科技（湖北）有限公司 | The holographic biochemistry high-valued extraction separation method of physics coupled system of Chinese medicine and Magnolia cortex P.E |
| CN107372966A (en) * | 2017-08-21 | 2017-11-24 | 紫云自治县红花茶业种植有限公司 | A kind of balloonflower root jasmine tea and preparation method thereof |
| CN115067534A (en) * | 2022-07-11 | 2022-09-20 | 湖北中烟工业有限责任公司 | Preparation method of vine tea extract for cigarettes |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN102617667B (en) | Method for simultaneously preparing total caffeoylquinic acid and stevioside by taking stevia as raw material | |
| CN103223018B (en) | Flos Osmanthi Fragrantis polyphenol extract and its production and use | |
| CN100590109C (en) | Technique for extracting cynamorlum herba cistanches medicinal materials effective component | |
| CN101942355A (en) | Comprehensive extraction method for extracting tea seed oil, tea saponin and tea seed polysaccharide from tea seeds or camellia seeds | |
| CN102225091A (en) | Method for preparing barbat skullcap total polyphenol | |
| CN104306443B (en) | A kind of method of oil camphor tree leaf comprehensive utilization | |
| CN102127140A (en) | Method for combinedly extracting Morroniside, dogwood polysaccharide and ursolic acid from dogwood | |
| CN101008022B (en) | Preparation method of scutellaria root flavone general aglycone extract | |
| CN103976453A (en) | Chuzhou chrysanthemum extract, solid beverage, lozenges and food additive as well as preparation method of Chuzhou chrysanthemum extract | |
| CN102304501A (en) | Complex enzyme preparation and application and method thereof for extracting plant polysaccharides by using same | |
| CN101570581A (en) | Method for comprehensively extracting pueraria polysaccharide and flavone | |
| CN102731592B (en) | A kind of method extracting oleuropein and Tridemethylsciadopitysin from olive leaf | |
| CN105670795A (en) | Peppermint oil extraction method | |
| CN102716208A (en) | Preparation method for general flavone extract from seed coats of peony | |
| CN103356740B (en) | Preparation method of baicalein and scutellaria baicalensis flavone total-aglycone extractives | |
| CN103830292A (en) | Apocynum flavonoid extract and preparation method thereof | |
| CN101982184B (en) | Preparation method of taraxacum extract | |
| CN101696381B (en) | Novel process for preparing highland barley flavone extract and application thereof in health wine | |
| CN102432419B (en) | Method for extracting and separating beta-elemene from Eupatorium adenophorum | |
| CN102432420B (en) | Method for extracting and separating beta-elemene from Lantana camara | |
| CN102964462B (en) | Wedelia prostrate polysaccharide as well as preparation method and application of wedelia prostrate polysaccharide | |
| CN108126000A (en) | Arasaponin extracts preparation method in fresh Radix Notoginseng | |
| CN101129415A (en) | Refined Chinese caterpillar fungus powder and method of preparing the same | |
| CN104706688A (en) | Method for preparing effective parts of nutmeg total lignanoids | |
| CN106800676A (en) | The extracting method of dendrobium polysaccharide |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C02 | Deemed withdrawal of patent application after publication (patent law 2001) | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20111026 |