CN101810647B - Method for supercritical CO2 extraction of total flavonoids of athyrium multidentatum ching - Google Patents

Method for supercritical CO2 extraction of total flavonoids of athyrium multidentatum ching Download PDF

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CN101810647B
CN101810647B CN2010101438621A CN201010143862A CN101810647B CN 101810647 B CN101810647 B CN 101810647B CN 2010101438621 A CN2010101438621 A CN 2010101438621A CN 201010143862 A CN201010143862 A CN 201010143862A CN 101810647 B CN101810647 B CN 101810647B
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supercritical
extraction
female dragon
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monkey leg
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CN101810647A (en
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刘冬梅
盛继文
李凤荣
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Weifang Medical University
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刘冬梅
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Abstract

The invention relates to a method for the supercritical CO2 extraction of the total flavonoids of athyrium multidentatum (doll.) ching. The method comprises the following steps: grinding the whole grass of athyrium multidentatum (doll.) ching; placing the ground whole grass of athyrium multidentatum (doll.) ching in the extraction kettle of a supercritical extraction device using supercritical CO2 as solvent and 60%-100% ethanol as entrainer with the flow ratio between the entrainer and the solvent being 5% to 25%; adjusting the extraction kettle until the extraction pressure is controlled within 25MPa to 35MPa, the temperature is controlled within 40 to 50 DEG C, and the flow rate of CO2 is controlled within 5L/h to 20L/h; extracting for 3h to 5h; separating and resolving the extracted whole grass powder of athyrium multidentatum (doll.) ching in a separation kettle using supercritical CO2 as solvent; and adjusting the separation kettle until the separating/resolving pressure is controlled within 8MPa to 10MPa, the temperature is controlled within 40 to 50 DEG C and the flow rate of the CO2 is controlled within 5L/h to 20L/h to obtain the brown pasty whole grass total flavonoids of athyrium multidentatum (doll.) ching. By using the technical parameter to carry out the supercritical extraction and further carrying out the separating and resolving processes in the separation kettle, the method of the invention has the advantages that the average yield reaches 14.04%, the content of impurities is low, and the operating conditions are mild and controllable.

Description

A kind of supercritical CO＜sub of monkey leg female dragon general flavone〉2＜/sub〉extracting process
Technical field
The present invention relates to a kind of extracting method of effective components of Chinese medicinal, specifically, relate to a kind of supercritical CO of monkey leg female dragon general flavone 2Extracting process belongs to technical field of traditional Chinese medicines.
Background technology
Pteridophyte claims pteridophyte again, is that a group all has multifarious cryptogam aspect germplasm and the metabolite, the pteridophyte aboundresources, the whole world has 12000 kinds approximately, in kind surplus state-owned 2600.Medicinal pteridophyte has wide biological activity, studies show that chemical compositions such as the flavones that contains in the pteridophyte, terpene, phenols, polysaccharide have antitumor action, have stronger inhibitory action to kinds of tumors.
Monkey leg female dragon (Athyrium Multidentatum (Doll.) Ching.) is Athyriaceae (Athyriaceae) plant, have another name called athyrium multidenatum Ching, many toothed lady fern, monkey leg, it is a kind of perennial pteridophyte, its fist shape tender leaf and root-like stock edible, pluck spring, can coldly boil in water for a while, then dress with soy, vinegar, etc., cold and dressed with sauce or stir-fry and eat, also can add salt marsh or shine into dry vegetalbe with shredded meat, delicious flavour, unique flavor are a kind of main hill dishes of Changbaishan area.Monkey leg female dragon is not only edible, and is also pharmaceutically acceptable, for of Chinese medicine rhizome of cyrtomium commonly uses kind.Monkey leg female dragon rhizome and herb all can be used as medicine, distinguish the flavor of sweet, little hardship, puckery cold, can calm the nerves, step-down, diuresis, antipyretic-antalgic, wind dispelling are wet etc., but and expelling parasite, stop blooding, control snakeworm and bite etc., be a class important " medicine, food dual-purpose " pteridophyte, its nutritional labeling and medicinal efficacy and fiddlehead are suitable.Often eat and to treat diseases such as hypertension, giddy, uterine hemorrhage, arthritis, and measles, influenza are had prevention effect.In addition, contain abundant lysine in the many toothed lady fern, can promote the formation of skeleton development and tooth, suppress viral infection etc., especially to the very big meaning of being supplemented with of infant, maternal nutritional.Medicinal pteridophyte has BA widely, and excellent antibiotic, antimicrobial, antiviral, anti-oxidant, antimalarial, diuresis, step-down and effect such as antitumor are arranged.Have the effect of expelling parasite, clearing heat and detoxicating, diuresis, hemostasis as the Chinese medicine rhizome of cyrtomium, be used for the treatment of dysentery, swelling and pain relieving, traumatism and bleeding, ascarifuge, sore furuncle and compatibility and treat various cancers etc.
Paper and the patent report to monkey leg female dragon flavones extracting method do not found in literature search as yet.Application number is 200610135368.4 Chinese invention patent proposition pteridophyte flavones supercritical extraction method: the fern root, stem, the leaf dried powder that crush are placed the supercritical extract cylinder, use supercritical CO 2Be solvent, 60-90% ethanol is done entrainer, and extracting pressure is 8-50MPa, the extraction of temperature 35-50 ℃ of condition, and extraction time 3-5h, and be that example is illustrated the concrete operations step with the Stenoloma chusana.Because flavone compound polarity differs bigger, does not have a kind of general supercritical extract entrainer that is applicable to flavones.The approximate range of above-mentioned patent provides the pteridophyte flavones when carrying out supercritical extract entrainer concentration, temperature, pressure, because pteridophyte belongs to the difference between kind in geographical growing environment, section, cause pteridophyte between institutional framework, chemical composition composition and content, to there are differences, actual operating condition difference when carrying out pteridophyte flavone compound supercritical extract is difficult to effectively implement and obtain satisfied effect of extracting according to the foregoing invention patent.
Summary of the invention
The problem to be solved in the present invention is at above deficiency, proposes a kind of monkey leg female dragon general flavone supercritical CO 2Extracting process, the general flavone productive rate height that utilizes this method to extract is impure few.
For solving above technical problem, the technical solution adopted in the present invention is: a kind of supercritical CO of monkey leg female dragon general flavone 2Extracting process is characterized in that: described extracting process may further comprise the steps:
1) the monkey leg female dragon herb of drying is pulverized in pulverizer, the monkey leg female dragon herb powder after pulverizing is placed the extraction kettle of supercritical extract instrument;
2) use supercritical CO 2As solvent, concentration is that the ethanol of 60%-100% is done entrainer, adopts continuous pump input mode to add ethanol, and the flow-rate ratio of entrainer and solvent is 5-25%;
3) regulate extraction kettle, extracting pressure is controlled at 25-35MPa, temperature is controlled at 40-50 ℃, CO 2Flow-control extracts time 3-5h at 5-20L/h;
4) the monkey leg female dragon herb powder after will extracting places separating still to separate to resolve, use supercritical CO 2As solvent, regulate separating still, make separation resolve pressure and be controlled at 8-10MPa, temperature is controlled at 40-50 ℃, CO 2Flow-control gets brown paste monkey leg female dragon herb total flavonoids at 5-20L/h.
As further improvement in the technical proposal:
Described concentration of ethanol is 80%.
The flow-rate ratio of described entrainer and solvent is 20%.
Described extracting pressure is 30MPa.
Described extraction temperature is 45 ℃.
In the described extraction step, CO 2Flow is 15L/h.
The described extraction time is 5h.
Described separation resolution temperature is 45 ℃.
In the described separation analyzing step, CO 2Flow is 15L/h.
The present invention adopts above technical scheme, compared with prior art, have the following advantages: place extraction kettle to adopt above technical parameter to carry out supercritical extract monkey leg female dragon herb, place separating still to adopt above technical parameter to separate parsing again, average yield can reach 14.04%, impurity is few, operating condition gentleness, controlled.
The present invention is described in detail below in conjunction with embodiment.
The specific embodiment
Embodiment, experiment 1, a kind of supercritical CO of monkey leg female dragon general flavone 2Extracting process may further comprise the steps:
1) the monkey leg female dragon herb of drying is pulverized in pulverizer, the monkey leg female dragon herb powder after pulverizing is placed the extraction kettle of supercritical extract instrument;
2) use supercritical CO 2As solvent, select for use ethanol to do entrainer, the occurrence of concentration of alcohol adopts continuous pump input mode to add ethanol as shown in table 1,2, and the flow-rate ratio of entrainer and solvent is 20%;
3) regulate extraction kettle, control extracting pressure, extraction temperature and extraction time, CO 2Flow-control is at 15L/h;
Change respectively extracting pressure, extraction temperature and extraction time carry out nine times the test, extracting pressure, extraction temperature and the occurrence of extraction time are as shown in table 1,2;
In the described table: wherein A is an extracting pressure, units MPa; B is an extraction temperature, unit ℃; C is the extraction time, the h of unit; D is an entrainer concentration, the % of unit.
4) the monkey leg female dragon herb powder after will extracting places separating still to separate to resolve, use supercritical CO 2As solvent, regulate separating still, make separation resolve pressure and be controlled at 8MPa, separate resolution temperature and be controlled at 45 ℃, CO 2Flow-control gets brown paste monkey leg female dragon herb total flavonoids at 15L/h.
With monkey leg female dragon general flavone extraction yield is index, and table 1 is a supercritical extraction process factor level table.
Carry out the test of 4 factors, 3 horizontal quadratures according to table 1 pair extracting pressure, temperature, extraction time and entrainer concentration, according to L 9(3 4) surface condition experimentizes.This experiment is a foundation with the trial test result.Table 2 is the supercritical extraction process orthogonal experiments;
Table 3 is the supercritical extraction process The results of analysis of variance.
Table 1
Level Factor
A B C D
1 25 40 3 100
2 30 45 4 80
3 35 50 5 60
Table 2
Figure GSA00000080155000041
Table 3
Soruces of variation Sum of square of deviations The free degree The F ratio The F critical value Conspicuousness
A 18.736 2 49.830 19.000 *
B 0.376 2 1.000 19.000
C 12.682 2 33.729 19.000 *
D 9.669 2 25.715 19.000 *
Error 0.38 2
The supercritical extraction process ANOVA showed significant of table 3, the factor that monkey leg female dragon general flavone recovery rate is had the greatest impact is A extracting pressure, C extraction time, D entrainer concentration, the B extraction temperature is not remarkable to the extraction yield influence.Monkey leg female dragon general flavone supercritical CO 2The extraction process best of breed is A 2B 2C 3D 2, i.e. extracting pressure 30MPa, 45 ℃ of extraction temperature, extraction time 5h and entrainer concentration 80%, this selection process operating condition gentleness is applicable to the large-scale industrial production of monkey leg female dragon general flavone.
Experiment 2, the checking of monkey leg female dragon general flavone supercritical extraction process.
A kind of supercritical CO of monkey leg female dragon general flavone 2Extracting process may further comprise the steps:
1) the monkey leg female dragon herb of drying is pulverized in pulverizer, the monkey leg female dragon herb powder after pulverizing is placed the extraction kettle of supercritical extract instrument;
2) use supercritical CO 2As solvent, concentration is that 80% ethanol is done entrainer, adopts continuous pump input mode to add ethanol, and the flow-rate ratio of entrainer and solvent is 20%;
3) regulate extraction kettle, extracting pressure is controlled at 30MPa, extraction temperature is controlled at 45 ℃, CO 2Flow-control extracts time 5h at 15L/h;
4) the monkey leg female dragon herb powder after will extracting places separating still to separate to resolve, use supercritical CO 2As solvent, regulate separating still, make separation resolve pressure and be controlled at 8MPa, separate resolution temperature and be controlled at 45 ℃, CO 2Flow-control gets brown paste monkey leg female dragon herb total flavonoids at 15L/h.
Carry out three experiments according to above method, the extraction yield of experiment is 14.25% for the first time, and the extraction yield of experiment is 13.57% for the second time, and Shi Yan extraction yield is 14.31% for the third time, and average extraction yield is 14.04%, and RSD is 2.92%.
This experiment shows, is 30MPa in extracting pressure, 45 ℃ of extraction temperature, and extraction time 5h, under the extraction conditions of entrainer concentration 80%, the average extraction yield of monkey leg female dragon general flavone can reach 14.04%, and extraction yield is higher, and effect is better.
Experiment 3, the entrainer consumption is to the influence of monkey leg female dragon general flavone extraction yield.
A kind of supercritical CO of monkey leg female dragon general flavone 2Extracting process may further comprise the steps:
1) the monkey leg female dragon herb of drying is pulverized in pulverizer, the monkey leg female dragon herb powder after pulverizing is placed the extraction kettle of supercritical extract instrument;
2) use supercritical CO 2As solvent, concentration is that 80% ethanol is done entrainer, adopts continuous pump input mode to add ethanol;
3) regulate extraction kettle, extracting pressure is controlled at 30MPa, extraction temperature is controlled at 45 ℃, CO 2Flow-control extracts time 5h at 15L/h;
4) the monkey leg female dragon herb powder after will extracting places separating still to separate to resolve, use supercritical CO 2As solvent, regulate separating still, make separation resolve pressure and be controlled at 8MPa, separate resolution temperature and be controlled at 45 ℃, CO 2Flow-control gets brown paste monkey leg female dragon herb total flavonoids at 15L/h.
Get entrainer/CO 2Flow-rate ratio is 5%, 10%, 15%, 20% and 25%, experimentizes respectively according to above method, and each experiment is carried out three times, the extraction yield and the calculating mean value of the each experiment of record, and result such as following table:
Figure GSA00000080155000061
The result shows, along with entrainer/CO 2The increase of flow-rate ratio, extraction yield increases, entrainer/CO 2Flow-rate ratio is that 20% o'clock extraction yield is the highest, continues to increase entrainer/CO 2Flow-rate ratio, extraction yield reduces.
Experiment 4, CO 2Flow is to the influence of monkey leg female dragon general flavone extraction yield.
A kind of supercritical CO of monkey leg female dragon general flavone 2Extracting process may further comprise the steps:
1) the monkey leg female dragon herb of drying is pulverized in pulverizer, the monkey leg female dragon herb powder after pulverizing is placed the extraction kettle of supercritical extract instrument;
2) use supercritical CO 2As solvent, concentration is that 80% ethanol is done entrainer, adopts continuous pump input mode to add ethanol, and the flow-rate ratio of entrainer and solvent is 20%;
3) regulate extraction kettle, extracting pressure is controlled at 30MPa, extraction temperature is controlled at 45 ℃, extraction time 5h;
4) the monkey leg female dragon herb powder after will extracting places separating still to separate to resolve, use supercritical CO 2As solvent, regulate separating still, make separation resolve pressure and be controlled at 8MPa, separate resolution temperature and be controlled at 45 ℃, get brown paste monkey leg female dragon herb total flavonoids.
Get CO in extraction and the separating step 2Flow is 5L/h, 15L/h and 20L/h, experimentizes respectively according to above method, and each experiment is carried out three times, the extraction yield and the calculating mean value of the each experiment of record, and result such as following table:
Figure GSA00000080155000071
Above result changes supercritical extract CO as can be seen 2Flow, monkey leg female dragon general flavone extraction yield is had a significant effect.CO 2Flow increases, CO 2Contact reinforcement with the mass transfer in the material powder, help the stripping of flavones, along with flow continues to increase CO 2Shorten the extraction yield step-down time of contact with material powder.CO as can be seen from the table 2Extraction yield was the highest when flow was 15L/h.
Experiment 5, the separating still temperature is to the influence of monkey leg female dragon general flavone extraction yield.
A kind of supercritical CO of monkey leg female dragon general flavone 2Extracting process may further comprise the steps:
1) the monkey leg female dragon herb of drying is pulverized in pulverizer, the monkey leg female dragon herb powder after pulverizing is placed the extraction kettle of supercritical extract instrument;
2) use supercritical CO 2As solvent, concentration is that 80% ethanol is done entrainer, adopts continuous pump input mode to add ethanol, and the flow-rate ratio of entrainer and solvent is 20%;
3) regulate extraction kettle, extracting pressure is controlled at 30MPa, extraction temperature is controlled at 45 ℃, CO 2Flow-control extracts time 5h at 15L/h;
4) the monkey leg female dragon herb powder after will extracting places separating still to separate to resolve, use supercritical CO 2As solvent, regulate separating still, make separation resolve pressure and be controlled at 8MPa, CO 2Flow-control gets brown paste monkey leg female dragon herb total flavonoids at 15L/h.
Getting the separation resolution temperature is 40 ℃, 45 ℃ and 50 ℃, experimentizes respectively according to above method, and each experiment is carried out three times, the extraction yield and the calculating mean value of the each experiment of record, and result such as following table:
Figure GSA00000080155000072
Separate the resolution temperature result of study and show that the rising that separates resolution temperature helps improving the flavones extraction yield, no longer increase along with temperature continues the rising extraction yield, extraction yield was the highest when the separation resolution temperature was 45 ℃.
Experiment 6, separating still pressure is to the influence of monkey leg female dragon general flavone extraction yield.
A kind of supercritical CO of monkey leg female dragon general flavone 2Extracting process may further comprise the steps:
1) the monkey leg female dragon herb of drying is pulverized in pulverizer, the monkey leg female dragon herb powder after pulverizing is placed the extraction kettle of supercritical extract instrument;
2) use supercritical CO 2As solvent, concentration is that 80% ethanol is done entrainer, adopts continuous pump input mode to add ethanol, and the flow-rate ratio of entrainer and solvent is 20%;
3) regulate extraction kettle, extracting pressure is controlled at 30MPa, extraction temperature is controlled at 45 ℃, CO 2Flow-control extracts time 5h at 15L/h;
4) the monkey leg female dragon herb powder after will extracting places separating still to separate to resolve, use supercritical CO 2As solvent, regulate separating still, make the separation resolution temperature be controlled at 45 ℃, CO 2Flow-control gets brown paste monkey leg female dragon herb total flavonoids at 15L/h.
Getting separation parsing pressure is 8MPa, 9MPa and 10MPa, experimentizes respectively according to above method, and each experiment is carried out three times, the extraction yield and the calculating mean value of the each experiment of record, and result such as following table:
Figure GSA00000080155000081
Experimental result shows, resolves pressure in the separation resolving to the extraction yield influence not quite, extracting pressure and the more little conserve energy that helps more of parsing pressure difference value in operating process.The selected 8-10MPa of this experiment resolves pressure is not had obvious influence to extraction yield, simultaneously little with the extracting pressure difference, and flavones is separated preferably with material powder in this resolves pressure limit, and impurity content is few, the extraction yield height.

Claims (9)

1. the supercritical CO of a monkey leg female dragon general flavone 2Extracting process is characterized in that: described extracting process may further comprise the steps:
1) the monkey leg female dragon herb of drying is pulverized in pulverizer, the monkey leg female dragon herb powder after pulverizing is placed the extraction kettle of supercritical extract instrument;
2) use supercritical CO 2As solvent, concentration is that the ethanol of 60%-100% is done entrainer, adopts continuous pump input mode to add ethanol, and the flow-rate ratio of entrainer and solvent is 5-25%;
3) regulate extraction kettle, extracting pressure is controlled at 25-35MPa, temperature is controlled at 40-50 ℃, CO 2Flow-control extracts time 3-5h at 5-20L/h;
4) the monkey leg female dragon herb powder after will extracting places separating still to separate to resolve, use supercritical CO 2As solvent, regulate separating still, make separation resolve pressure and be controlled at 8-10MPa, temperature is controlled at 40-50 ℃, CO 2Flow-control gets brown paste monkey leg female dragon herb total flavonoids at 5-20L/h.
2. the supercritical CO of a kind of monkey leg female dragon general flavone as claimed in claim 1 2Extracting process is characterized in that: described concentration of ethanol is 80%.
3. the supercritical CO of a kind of monkey leg female dragon general flavone as claimed in claim 1 2Extracting process is characterized in that: the flow-rate ratio of described entrainer and solvent is 20%.
4. the supercritical CO of a kind of monkey leg female dragon general flavone as claimed in claim 1 2Extracting process is characterized in that: described extracting pressure is 30MPa.
5. the supercritical CO of a kind of monkey leg female dragon general flavone as claimed in claim 1 2Extracting process is characterized in that: described extraction temperature is 45 ℃.
6. the supercritical CO of a kind of monkey leg female dragon general flavone as claimed in claim 1 2Extracting process is characterized in that: in the described extraction step, and CO 2Flow is 15L/h.
7. the supercritical CO of a kind of monkey leg female dragon general flavone as claimed in claim 1 2Extracting process is characterized in that: the described extraction time is 5h.
8. the supercritical CO of a kind of monkey leg female dragon general flavone as claimed in claim 1 2Extracting process is characterized in that: described separation resolution temperature is 45 ℃.
9. the supercritical CO of a kind of monkey leg female dragon general flavone as claimed in claim 1 2Extracting process is characterized in that: in the described separation analyzing step, and CO 2Flow is 15L/h.
CN2010101438621A 2010-04-12 2010-04-12 Method for supercritical CO2 extraction of total flavonoids of athyrium multidentatum ching Expired - Fee Related CN101810647B (en)

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CN100999511A (en) * 2006-12-22 2007-07-18 洪伟 Supercritical extracting of fern flavone and preparation process of perflavone green tea

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CN100999511A (en) * 2006-12-22 2007-07-18 洪伟 Supercritical extracting of fern flavone and preparation process of perflavone green tea

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Title
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