CN113230314A - Method for extracting tartary buckwheat flavone - Google Patents
Method for extracting tartary buckwheat flavone Download PDFInfo
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- CN113230314A CN113230314A CN202110600739.6A CN202110600739A CN113230314A CN 113230314 A CN113230314 A CN 113230314A CN 202110600739 A CN202110600739 A CN 202110600739A CN 113230314 A CN113230314 A CN 113230314A
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- tartary buckwheat
- extraction
- immobilized enzyme
- flavone
- mixed material
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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)
- A61K36/70—Polygonaceae (Buckwheat family), e.g. spineflower or dock
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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
- A61K2236/10—Preparation or pretreatment of starting material
- A61K2236/15—Preparation or pretreatment of starting material involving mechanical treatment, e.g. chopping up, cutting or grinding
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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
- A61K2236/10—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
-
- 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
- A61K2236/53—Liquid-solid separation, e.g. centrifugation, sedimentation or crystallization
Abstract
The invention discloses a method for extracting tartary buckwheat flavone, which comprises the following steps: drying and crushing the tartary buckwheat seeds to obtain tartary buckwheat powder; mixing tartary buckwheat powder with immobilized enzyme to obtain a mixed material, wherein the immobilized enzyme comprises cellulase, pectinase and hemicellulase; putting the mixed material into an organic solution for extraction and filtration, and collecting filtrate; evaporating, concentrating, centrifuging, and drying the filtrate to obtain tartary buckwheat flavone; according to the extraction method, the immobilized enzyme is added, so that the cellulose and pectin in the tartary buckwheat seeds can be destroyed, the precipitation of flavone in the tartary buckwheat can be promoted, and the pectin mucus is prevented from being wrapped to inhibit the extraction of effective components; in addition, the invention obviously improves the extraction rate of the buckwheat flavone by limiting the type and the dosage of the immobilized enzyme and the extraction temperature.
Description
Technical Field
The invention relates to the technical field of extraction of buckwheat flavonoids, and particularly relates to an extraction method of buckwheat flavonoids.
Background
Fagopyrum tataricum (F. tataricum) belongs to Polygonaceae (Polygonaceae) Fagopyrum genus (Fagopyrum Mil) annual herbaceous plant. The tartary buckwheat is rich in nutrition, and the contents of protein, fat, vitamins and trace elements are generally higher than those of rice, wheat and corn. The tartary buckwheat also contains special nutrients such as rutin which are not possessed by other grain crops, and has the medical functions of assisting in treating cardiovascular and cerebrovascular diseases, hypertension, diabetes, cancer, clearing heat, removing toxicity, diminishing inflammation and the like. In recent years, along with the improvement of living standard of people, the development and utilization of tartary buckwheat has raised the trend of heat in the food and medicine world in China, and the development of health foods such as tartary buckwheat tea, noodles and snacks is concerned by food processing enterprises at home and abroad.
The tartary buckwheat has the effects of reducing blood pressure, reducing blood sugar and the like, active substances in the tartary buckwheat are mainly tartary buckwheat flavone, and the main components of the tartary buckwheat flavone comprise quercetin, rutin and the like, so that the tartary buckwheat flavone has the effects of preventing arteriosclerosis, inhibiting malignant cell growth, inhibiting platelet aggregation and the like; at present, most of the extraction methods of the tartary buckwheat flavone directly adopt an organic solvent for reflux extraction, and the extraction efficiency and the purity are low.
Disclosure of Invention
The invention aims to provide an extraction method of buckwheat flavonoids, which can fully extract flavonoids in buckwheat seeds and effectively improve the extraction rate of buckwheat flavonoids and the purity of extracted products.
In order to achieve the above purpose of the present invention, the following technical solutions are adopted:
the invention provides a method for extracting tartary buckwheat flavone, which comprises the following steps:
(a) drying and crushing the tartary buckwheat seeds to obtain tartary buckwheat powder;
(b) mixing tartary buckwheat powder with immobilized enzyme to obtain a mixed material, wherein the immobilized enzyme comprises cellulase, pectinase and hemicellulase;
(c) putting the mixed material into an organic solution for extraction and filtration, and collecting filtrate;
(d) evaporating, concentrating, centrifuging, and drying the filtrate to obtain tartary buckwheat flavone.
Preferably, the grain size of the tartary buckwheat powder is 100-200 meshes.
Preferably, the mass ratio of the tartary buckwheat powder to the immobilized enzyme is 100: 1-5.
Preferably, the immobilized enzyme is composed of the following components in parts by weight:
10-20 parts of cellulase, 1-5 parts of pectinase and 8-12 parts of hemicellulase.
Preferably, the activity of the cellulase is 1500-2000U/g, the activity of the pectinase is 1000-2000U/g, and the activity of the hemicellulase is 2000-3000U/g.
Preferably, the extraction temperature is 30-45 ℃, the extraction time is 3-5 h, and the pH is 3.5-5.5.
Preferably, the mass ratio of the mixed material to the organic solution is 1: 8-12; the organic solution is an ethanol solution with the mass concentration of 40-50%.
Preferably, the evaporation concentration is carried out to 0.4-0.5 times of the volume of the filtrate.
Preferably, the centrifugal rotating speed is 8000-12000 r/min, and the centrifugal time is 20-25 min.
Preferably, the drying temperature in step (a) and step (d) is not more than 50 ℃.
Compared with the prior art, the invention has the beneficial effects that at least:
according to the extraction method, the immobilized enzyme is added, so that the cellulose and pectin in the tartary buckwheat seeds can be destroyed, the precipitation of flavone in the tartary buckwheat can be promoted, and the pectin mucus is prevented from being wrapped to inhibit the extraction of effective components; in addition, the invention obviously improves the extraction rate of the buckwheat flavone by limiting the type and the dosage of the immobilized enzyme and the extraction temperature.
Detailed Description
The following describes embodiments of the present invention in detail with reference to the following embodiments. The following examples are only for illustrating the technical solutions of the present invention more clearly, and therefore are only examples, and the protection scope of the present invention is not limited thereby.
It is to be noted that, unless otherwise specified, technical or scientific terms used herein shall have the ordinary meaning as understood by those skilled in the art to which the invention pertains.
The embodiment of the invention provides an extraction method of tartary buckwheat flavone, which comprises the following steps:
(a) drying and crushing the tartary buckwheat seeds to obtain tartary buckwheat powder;
(b) mixing tartary buckwheat powder with immobilized enzyme to obtain a mixed material, wherein the immobilized enzyme comprises cellulase, pectinase and hemicellulase;
(c) putting the mixed material into an organic solution for extraction and filtration, and collecting filtrate;
(d) evaporating, concentrating, centrifuging, and drying the filtrate to obtain tartary buckwheat flavone.
The extraction method can destroy cellulose and pectin in tartary buckwheat seeds, promote precipitation of flavone in tartary buckwheat, and prevent pectin mucus from wrapping to inhibit extraction of effective components by adding immobilized enzyme.
In order to better promote the extraction of the buckwheat flavone, further, the grain size of the buckwheat powder is 100-200 meshes; by limiting the particle size of the tartary buckwheat powder, the precipitation of the tartary buckwheat flavone can be better promoted, the extraction time is shortened, and the extraction rate is improved.
In the invention, the addition amount of the immobilized enzyme is not strictly limited, and preferably, the mass ratio of the tartary buckwheat powder to the immobilized enzyme is 100: 1-5; further, the immobilized enzyme comprises the following components in parts by weight:
10-20 parts of cellulase, 1-5 parts of pectinase and 8-12 parts of hemicellulase;
furthermore, the activity of the cellulase is 1500-2000U/g, the activity of the pectinase is 1000-2000U/g, and the activity of the hemicellulase is 2000-3000U/g.
According to the invention, the extraction of the buckwheat flavone can be better promoted by limiting the type, the dosage and the activity of the immobilized enzyme, and the extraction rate of the buckwheat flavone is remarkably improved.
In the invention, the control of the extraction parameters is not strictly limited and can be reasonably selected according to actual needs; preferably, the extraction temperature is 30-45 ℃, the extraction time is 3-5 h, and the pH is 3.5-5.5; further, the mass ratio of the mixed material to the organic solution is 1: 8-12; the organic solution is ethanol solution with the mass concentration of 40-50%. .
Through the specific selection of the organic solution and the control of extraction parameters, the activity of immobilized enzyme can be guaranteed, and the extraction of the tartary buckwheat flavone is promoted.
Further, evaporating and concentrating to 0.4-0.5 time of the volume of the filtrate.
Further, the centrifugal rotating speed is 8000-12000 r/min, and the centrifugal time is 20-25 min.
Further, the drying temperature in step (a) and step (d) does not exceed 50 ℃.
The technical solution of the present invention is further described in detail by the following specific examples.
Example 1
The embodiment is a method for extracting tartary buckwheat flavone, which comprises the following steps:
(a) drying and crushing the tartary buckwheat seeds at 45-50 ℃ to obtain 100-200 mesh tartary buckwheat powder;
(b) mixing the tartary buckwheat powder and an immobilized enzyme according to the mass ratio of 100: 1 of the tartary buckwheat powder to the immobilized enzyme to obtain a mixed material, wherein the immobilized enzyme consists of 20 parts of cellulase, 1 part of pectinase and 12 parts of hemicellulase, the activity of the cellulase is 2000U/g, the activity of the pectinase is 2000U/g, and the activity of the hemicellulase is 3000U/g;
(c) according to the mass ratio of the mixed material to the 40% ethanol solution of 1: 12, placing the mixed material in the 40% ethanol solution for extraction and filtration, and collecting filtrate, wherein the extraction temperature is 30 ℃, the time is 5h, and the pH is 5.5;
(d) evaporating the filtrate, concentrating to 0.47 times the volume of the filtrate, centrifuging at 10000r/min for 22min, collecting precipitate, and drying the precipitate at 45 deg.C to obtain tartary buckwheat flavone.
Example 2
The embodiment is a method for extracting tartary buckwheat flavone, which comprises the following steps:
(a) drying and crushing the tartary buckwheat seeds at 45-50 ℃ to obtain 100-200 mesh tartary buckwheat powder;
(b) mixing the tartary buckwheat powder and an immobilized enzyme according to the mass ratio of 100: 5 of the tartary buckwheat powder to the immobilized enzyme to obtain a mixed material, wherein the immobilized enzyme consists of 10 parts of cellulase, 5 parts of pectinase and 8 parts of hemicellulase, the activity of the cellulase is 2000U/g, the activity of the pectinase is 2000U/g, and the activity of the hemicellulase is 3000U/g;
(c) according to the mass ratio of the mixed material to the 50% ethanol solution of 1: 8, placing the mixed material in the 50% ethanol solution for extraction and filtration, and collecting filtrate, wherein the extraction temperature is 45 ℃, the time is 3h, and the pH is 3.5;
(d) evaporating the filtrate, concentrating to 0.46 times the volume of the filtrate, centrifuging at 10000r/min for 22min, collecting precipitate, and drying the precipitate at 45 deg.C to obtain tartary buckwheat flavone.
Example 3
The embodiment is a method for extracting tartary buckwheat flavone, which comprises the following steps:
(a) drying and crushing the tartary buckwheat seeds at 45-50 ℃ to obtain 100-200 mesh tartary buckwheat powder;
(b) mixing the tartary buckwheat powder and an immobilized enzyme according to the mass ratio of the tartary buckwheat powder to the immobilized enzyme of 100: 3 to obtain a mixed material, wherein the immobilized enzyme consists of 15 parts of cellulase, 3 parts of pectinase and 10 parts of hemicellulase, the activity of the cellulase is 2000U/g, the activity of the pectinase is 2000U/g, and the activity of the hemicellulase is 3000U/g;
(c) according to the mass ratio of the mixed material to the 45% ethanol solution of 1: 10, placing the mixed material in the 45% ethanol solution for extraction and filtration, and collecting filtrate, wherein the extraction temperature is 40 ℃, the time is 4h, and the pH is 4.5;
(d) evaporating the filtrate, concentrating to 0.42 times the filtrate volume, centrifuging at 10000r/min for 22min, collecting precipitate, and drying the precipitate at 45 deg.C to obtain tartary buckwheat flavone.
Comparative example 1
The comparative example is an extraction method of tartary buckwheat flavone, which is basically the same as the extraction method of the example 3, and the difference is only that the step (b) is as follows:
(b) the tartary buckwheat powder and the immobilized enzyme are mixed according to the mass ratio of 100: 3 of the tartary buckwheat powder to the immobilized enzyme to obtain a mixed material, wherein the immobilized enzyme is composed of 18 parts of cellulase and 10 parts of hemicellulase, the activity of the cellulase is 2000U/g, and the activity of the hemicellulase is 3000U/g.
Comparative example 2
The comparative example is an extraction method of tartary buckwheat flavone, which is basically the same as the extraction method of the example 3, and the difference is only that the step (c) is as follows:
(c) according to the mass ratio of the mixed material to the 45% ethanol solution of 1: 10, placing the mixed material in the 45% ethanol solution for extraction and filtration, and collecting filtrate, wherein the extraction temperature is 40 ℃, the time is 4h, and the pH is 6.
Examples of the experiments
Extracting the tartary buckwheat flavone in the tartary buckwheat seeds by adopting the extraction methods in the embodiment 3 and the comparison examples 1-2 respectively, and then calculating the yield according to the tartary buckwheat flavone/tartary buckwheat seeds multiplied by 100%; the calculation results are shown in table 1:
the purity of the tartary buckwheat flavone extracted by different methods is measured by adopting a spectrophotometry method, and the measurement result is shown in table 1:
TABLE 1 yield and purity of Tartary buckwheat flavones
| Group of | Example 3 | Comparative example 1 | Comparative example 2 |
| Yield of the product | 3.26％ | 2.71％ | 2.95％ |
| Purity of | 76.4％ | 78.3％ | 73.4％ |
As can be seen from the data in Table 1:
the extraction method provided by the embodiment of the application can be used for better extracting the tartary buckwheat flavone in the tartary buckwheat seeds, and the extraction rate of the tartary buckwheat flavone can be improved.
Finally, it should be noted that: the above embodiments are only used to illustrate the technical solution of the present invention, and not to limit the same; while the invention has been described in detail and with reference to the foregoing embodiments, it will be understood by those skilled in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some or all of the technical features may be equivalently replaced; such modifications and substitutions do not depart from the spirit and scope of the present invention, and they should be construed as being included in the following claims and description.
Claims (10)
1. The method for extracting the tartary buckwheat flavone is characterized by comprising the following steps:
(a) drying and crushing the tartary buckwheat seeds to obtain tartary buckwheat powder;
(b) mixing tartary buckwheat powder with immobilized enzyme to obtain a mixed material, wherein the immobilized enzyme comprises cellulase, pectinase and hemicellulase;
(c) putting the mixed material into an organic solution for extraction and filtration, and collecting filtrate;
(d) evaporating, concentrating, centrifuging, and drying the filtrate to obtain tartary buckwheat flavone.
2. The extraction method according to claim 1, wherein the particle size of the tartary buckwheat powder is 100-200 meshes.
3. The extraction method according to claim 1, wherein the mass ratio of the tartary buckwheat powder to the immobilized enzyme is 100: 1-5.
4. The extraction method according to claim 1, wherein the immobilized enzyme is composed of the following components in parts by weight:
10-20 parts of cellulase, 1-5 parts of pectinase and 8-12 parts of hemicellulase.
5. The extraction method according to claim 1 or 4, wherein the cellulase activity is 1500-2000U/g, the pectinase activity is 1000-2000U/g, and the hemicellulase activity is 2000-3000U/g.
6. The extraction method according to claim 1, wherein the extraction temperature is 30-45 ℃, the extraction time is 3-5 h, and the pH is 3.5-5.5.
7. The extraction method according to claim 1, wherein the mass ratio of the mixed material to the organic solution is 1: 8-12; the organic solution is an ethanol solution with the mass concentration of 40-50%.
8. The extraction method according to claim 1, wherein the evaporation is performed to a volume of 0.4 to 0.5 times of the volume of the filtrate.
9. The extraction method according to claim 1, wherein the centrifugation speed is 8000 to 12000r/min, and the centrifugation time is 20 to 25 min.
10. The extraction process according to claim 1, wherein the drying temperature in step (a) and step (d) is not more than 50 ℃.
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| CN202110600739.6A CN113230314B (en) | 2021-05-31 | 2021-05-31 | Method for extracting tartary buckwheat flavone |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115316470A (en) * | 2022-08-26 | 2022-11-11 | 云南八凯生物科技有限公司 | Instant tartary buckwheat tea and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101366830A (en) * | 2008-09-25 | 2009-02-18 | 成都大学 | Tartary buckwheat biological flavone effervescent tablet and preparation method thereof |
| CN103446254A (en) * | 2013-08-13 | 2013-12-18 | 西北大学 | Embedding method of buckwheat flavonoids |
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- 2021-05-31 CN CN202110600739.6A patent/CN113230314B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101366830A (en) * | 2008-09-25 | 2009-02-18 | 成都大学 | Tartary buckwheat biological flavone effervescent tablet and preparation method thereof |
| CN103446254A (en) * | 2013-08-13 | 2013-12-18 | 西北大学 | Embedding method of buckwheat flavonoids |
Non-Patent Citations (2)
| Title |
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| 曹娅等: "响应面优化苦荞黄酮超声波提取工艺", 《食品工业》 * |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115316470A (en) * | 2022-08-26 | 2022-11-11 | 云南八凯生物科技有限公司 | Instant tartary buckwheat tea and preparation method thereof |
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