CN102430063A - Process for extracting general flavone in reed leaves by supercritical CO2 method - Google Patents
Process for extracting general flavone in reed leaves by supercritical CO2 method Download PDFInfo
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- CN102430063A CN102430063A CN2011103801402A CN201110380140A CN102430063A CN 102430063 A CN102430063 A CN 102430063A CN 2011103801402 A CN2011103801402 A CN 2011103801402A CN 201110380140 A CN201110380140 A CN 201110380140A CN 102430063 A CN102430063 A CN 102430063A
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- total flavones
- folium phragmitis
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Abstract
The invention relates to a process for extracting general flavone in reed leaves by a supercritical CO2 method, belonging to the technical field of traditional Chinese medicines. The process comprises the following steps of: drying the reed leaves, crushing, sieving, putting reed leave powder in an extraction kettle of a supercritical extractor, adopting the supercritical CO2 as a solvent, adopting 60-80% alcohol as an entrainer, adjusting the extraction kettle, controlling the extraction pressure to be 25-35MPa, controlling the temperature to be 30-50 DEG C, controlling the flow of the CO2 to be 15L/h, controlling the extraction time to be 80-100min, and obtaining the brown pasty general flavone in the reed leaves. By adoption of the technical parameters, supercritical extraction has no pollution and toxic hazard, the extraction rate of the general flavone is high, the impurity is fewer and the condition is moderate and controllable.
Description
Technical field
The present invention relates to a kind of Chinese medicine extraction of effective components, specifically, relate to a kind of supercritical CO
2The technology of method extraction Folium Phragmitis total flavones belongs to technical field of Chinese medicines.
Background technology
Phragmites communis is the grass family herbaceos perennial, has extremely strong resistance and struggle for existence ability.The phragmites communis whole body all is precious, and wherein Flos Phragmitis, Caulis Phragmitis, Rhizoma Phragmitis, Folium Phragmitis, Germinatus Phragmitis all can be used as medicine.Folium Phragmitis is called for short Folium Phragmitis, and the spring, summer, autumn and winter all can gather, and wherein has a kind of Folium Phragmitis thin and wide, is bottle green at the beginning of 5 months, can be used for wrapping up rice tamale, is commonly called as ZONGYE.Compendium of Material Medica is all received the clauses and subclauses that Folium Phragmitis is arranged with " Chinese medicine voluminous dictionary ": nature and flavor are sweet, cold, nontoxic, cure mainly vomiting and dirarrhea, haematemesis, pain in the lung, carbuncle on the back, cholera vomiting, lung heat clearing preventing or arresting vomiting etc.Modern pharmacology confirms that the leaf of phragmites communis, flower, stem, root all contain abundant ingredient, therefore receives the attention on medical science, pharmacy and chemical boundary.Pharmacological actions such as the total flavones that from Folium Phragmitis, extracts has the blood pressure lowering blood fat reducing, increases coronary flow, heart tonifying, arrhythmia, antibacterial and antioxidation.The method of traditional extraction total flavones has soxhlet extraction, alcohol heating reflux method, problem such as these methods exist extraction time long, and the solvent for use amount is big, and extraction efficiency is low.
Do not see the supercritical CO that total flavones in the Folium Phragmitis is arranged in the literature search as yet
2The extracting process report.Application number is that 201010619905.9 Chinese invention patent adopts the method for conventional ethanol lixiviate to extract the Folium Phragmitis total flavones; Its method is characterised in that Folium Phragmitis is dry with the acid treatment final vacuum; Crushing screening; In powder, add ethanol extraction then, obtain the phragmites communis total flavonoids extract through rotary evaporation at last.Supercritical CO
2Abstraction technique is to develop chemical separating new technique rapidly over nearly 20 years in the world, and it is with characteristics such as pollution-free, separation efficiency height and caught people's attention.In recent years, because the advantage that supercritical extraction technique is had in the field of Chinese medicines, its application was flourish.Particularly the modernization of Chinese medicine or the modern production of traditional Chinese medicines action of country's enforcement more make it to become a big focus, become one of key technology of the modernization of Chinese medicine.Application number is the supercritical CO that 201010143862.1 Chinese invention patent proposes Athyrium multidentatum (Doll.) Ching female dragon total flavones
2Extracting process has provided the approximate range of process conditions such as entrainer concentration, extraction temperature, extracting pressure.But because different plants belong to the difference between kind in geographical growing environment, section; Cause different vegetable active compositions compositions and content aspect there are differences; Actual when carrying out the supercritical extraction total flavones operating condition different, according to the foregoing invention patent Folium Phragmitis total flavones is extracted and to be difficult to effectively implement and obtain promising result.
Summary of the invention
The object of the present invention is to provide the supercritical CO of total flavones in a kind of high efficiency extraction Folium Phragmitis
2Extraction process utilizes the Folium Phragmitis total flavones productive rate of this method extraction high, impure few.
The technical scheme that the present invention adopted is: a kind of supercritical CO
2The technology of method extraction Folium Phragmitis total flavones, it is characterized in that: said extracting process may further comprise the steps:
1), in pulverizer, pulverizes to behind the 20-80 order powder Folium Phragmitis powder being placed the extraction kettle of supercritical extraction appearance with the Folium Phragmitis 80g behind the vacuum drying;
2) use supercritical CO
2As solvent, concentration is that the ethanol of 50-80% is done entrainer;
3) regulate extraction kettle extracting pressure is controlled at 25-35MPa, temperature is controlled at 30-50 ℃, CO
2Flow-control is at 15L/h, and the extraction time is controlled at 80-100min, gets brown paste Folium Phragmitis total flavones.
According to a preferred implementation of the present invention, the reed powder powder stock granularity of using in the step (1) is 40 orders.
According to another preferred embodiment of the present invention, step (2) adopts 70% ethanol entrainer.
According to another preferred embodiment of the present invention, the supercritical CO that uses in the step (3)
2Flow is 15L/h.
According to another preferred embodiment of the present invention, the extracting pressure in the step (3) is 35MPa.
According to another preferred embodiment of the present invention, the extraction temperature in the step (3) is 40 ℃.
Compared with prior art, the invention has the advantages that, adopt supercritical CO
2Be solvent, pollution-free, nonhazardous, operating condition is gentle, and the total flavones productive rate of extraction is high.At concentration of alcohol is 70%, and the extraction time is 80min, and extraction temperature is 40 ℃, and extracting pressure is 35MPa, and phragmites communis total flavones productive rate is 0.97%.
Below in conjunction with embodiment the present invention is elaborated.
The specific embodiment
Embodiment 1
With adopting next fresh Folium Phragmitis process pretreatment: tap water cleans, and vacuum drying is pulverized, and sieves.Get powder 80g, add in the extraction kettle of supercritical extraction appearance.Use supercritical CO
2As solvent, concentration is that 70% ethanol is done entrainer, regulates extraction kettle extracting pressure is controlled at 35MPa, and temperature is controlled at 40 ℃, CO
2Flow-control is at 15L/h, and the extraction time is controlled at 80min, gets brown paste Folium Phragmitis total flavones, and phragmites communis total flavones productive rate is 0.97%.
Following method is adopted in the analysis of Folium Phragmitis total flavones: get 20mg rutin standard substance and place the 100mL volumetric flask, with 60% dissolve with ethanol standardize solution, get the rutin storing solution.Get that 50mL rutin storing solution is put into the volumetric flask of 100mL and with 30% ethanol standardize solution, must the rutin titer.Pipette the rutin standard solution 2.5mL of 0.1mg/mL, 5.0mL, 7.5mL, 10.0mL; 12.5mL, place the volumetric flask of 25mL respectively, add 5% sodium nitrite solution 0.75mL, shake up; After placing 10min, add 10% aluminum nitrate solution 0.75mL, shake up, place 10min; Add 1mol/L NaOH solution 10mL again, the alcoholic solution standardize solution with 30% is surveyed its absorbance at the 510nm place, gets standard curve.Regression equation is A
Absorbance=15.04C
Rutin concentration-0.018 (R=0.9999).
Accurately draw and extract appearance liquid 8mL for use in the volumetric flask of 25mL, ask extraction ratio according to the content of absorbance and regression equation calculation flavone and according to following formula.
Embodiment 2
With adopting next fresh Folium Phragmitis process pretreatment: tap water cleans, and vacuum drying is pulverized, and crosses 40 mesh sieves.Get powder 80g, add in the extraction kettle of supercritical extraction appearance.Use supercritical CO
2As solvent, CO
2Flow-control is at 15L/h.The concentration that changes extraction time, extraction temperature, extracting pressure and alcohol is respectively carried out nine experiments.The concrete numerical value of each factor such as table 1, shown in 2.
With Folium Phragmitis total flavones extraction ratio is index, and table 1 is a supercritical extraction process factor level table; Carry out the orthogonal experiment of four factors, three levels by table 1 pair entrainer concentration of ethanol, extraction time, extraction temperature, extracting pressure.This experiment is a foundation with the preliminary experiment result, and table 2 is the supercritical extraction process orthogonal experiments.
Table 1
Table 2
Analysis result shows in the table 2, and the extreme difference value R of extracting pressure is maximum in The above results, so secondly extracting pressure is extraction temperature to the having the greatest impact of extraction results, is concentration of ethanol once more, is the extraction time at last.The optimization extraction conditions is A
2B
1C
2D
3, promptly concentration of ethanol is 70%, and the extraction time is 80min, and extraction temperature is 40 ℃, and extracting pressure is 35MPa, the extraction ratio of Folium Phragmitis total flavones is about 0.97% with this understanding.
Claims (7)
1. supercritical CO
2The technology of method extraction Folium Phragmitis total flavones, it is characterized in that: said extracting process may further comprise the steps:
1), in pulverizer, pulverizes to behind the 20-80 order powder Folium Phragmitis powder being placed the extraction kettle of supercritical extraction appearance with the Folium Phragmitis 80g behind the vacuum drying;
2) use supercritical CO
2As solvent, concentration is that the ethanol of 50-80% is done entrainer;
3) regulate extraction kettle extracting pressure is controlled at 25-35MPa, temperature is controlled at 30-50 ℃, CO
2Flow-control is at 15L/h, and the extraction time is controlled at 80-100min, gets brown paste Folium Phragmitis total flavones.
2. a kind of supercritical CO as claimed in claim 1
2The technology of method extraction Folium Phragmitis total flavones, it is characterized in that: described concentration of alcohol is 70%.
3. a kind of supercritical CO as claimed in claim 1
2The technology of method extraction Folium Phragmitis total flavones, it is characterized in that: described extracting pressure is 35MPa.
4. a kind of supercritical CO as claimed in claim 1
2The technology of method extraction Folium Phragmitis total flavones, it is characterized in that: described extraction temperature is 40 ℃.
5. a kind of supercritical CO as claimed in claim 1
2The technology of method extraction Folium Phragmitis total flavones, it is characterized in that: the described extraction time is 80min.
6. a kind of supercritical CO as claimed in claim 1
2The technology of method extraction Folium Phragmitis total flavones, it is characterized in that: described raw material granularity is 40 orders.
7. the technology of a kind of supercritical CO 2 method extraction Folium Phragmitis total flavones as claimed in claim 1 is characterized in that: described CO
2Flow is 15L/h.
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| CN2011103801402A CN102430063A (en) | 2011-11-25 | 2011-11-25 | Process for extracting general flavone in reed leaves by supercritical CO2 method |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103099826A (en) * | 2012-12-31 | 2013-05-15 | 宁波泰康红豆杉生物工程有限公司 | Method for extracting taxusflavone from taxus chinensis leaves |
| CN104920984A (en) * | 2015-05-25 | 2015-09-23 | 郑桂富 | Reed leaf rice dumpling |
| CN106621451A (en) * | 2016-12-14 | 2017-05-10 | 西藏自治区农牧科学院畜牧兽医研究所 | Method for extracting active components in Indian azalea leaves by using ultra-critical CO2 |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101649253A (en) * | 2009-09-15 | 2010-02-17 | 盐城工学院 | Method for integrated application of bulrush biotic substance |
-
2011
- 2011-11-25 CN CN2011103801402A patent/CN102430063A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101649253A (en) * | 2009-09-15 | 2010-02-17 | 盐城工学院 | Method for integrated application of bulrush biotic substance |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103099826A (en) * | 2012-12-31 | 2013-05-15 | 宁波泰康红豆杉生物工程有限公司 | Method for extracting taxusflavone from taxus chinensis leaves |
| CN103099826B (en) * | 2012-12-31 | 2015-02-04 | 宁波泰康红豆杉生物工程有限公司 | Method for extracting taxusflavone from taxus chinensis leaves |
| CN104920984A (en) * | 2015-05-25 | 2015-09-23 | 郑桂富 | Reed leaf rice dumpling |
| CN106621451A (en) * | 2016-12-14 | 2017-05-10 | 西藏自治区农牧科学院畜牧兽医研究所 | Method for extracting active components in Indian azalea leaves by using ultra-critical CO2 |
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Application publication date: 20120502 |