CN111217784A - Method for extracting quercetin from plantain seeds - Google Patents
Method for extracting quercetin from plantain seeds Download PDFInfo
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- CN111217784A CN111217784A CN201811419102.1A CN201811419102A CN111217784A CN 111217784 A CN111217784 A CN 111217784A CN 201811419102 A CN201811419102 A CN 201811419102A CN 111217784 A CN111217784 A CN 111217784A
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- Prior art keywords
- semen plantaginis
- quercetin
- extraction
- extracting
- plantain
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D311/00—Heterocyclic compounds containing six-membered rings having one oxygen atom as the only hetero atom, condensed with other rings
- C07D311/02—Heterocyclic compounds containing six-membered rings having one oxygen atom as the only hetero atom, condensed with other rings ortho- or peri-condensed with carbocyclic rings or ring systems
- C07D311/04—Benzo[b]pyrans, not hydrogenated in the carbocyclic ring
- C07D311/22—Benzo[b]pyrans, not hydrogenated in the carbocyclic ring with oxygen or sulfur atoms directly attached in position 4
- C07D311/26—Benzo[b]pyrans, not hydrogenated in the carbocyclic ring with oxygen or sulfur atoms directly attached in position 4 with aromatic rings attached in position 2 or 3
- C07D311/28—Benzo[b]pyrans, not hydrogenated in the carbocyclic ring with oxygen or sulfur atoms directly attached in position 4 with aromatic rings attached in position 2 or 3 with aromatic rings attached in position 2 only
- C07D311/30—Benzo[b]pyrans, not hydrogenated in the carbocyclic ring with oxygen or sulfur atoms directly attached in position 4 with aromatic rings attached in position 2 or 3 with aromatic rings attached in position 2 only not hydrogenated in the hetero ring, e.g. flavones
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D311/00—Heterocyclic compounds containing six-membered rings having one oxygen atom as the only hetero atom, condensed with other rings
- C07D311/02—Heterocyclic compounds containing six-membered rings having one oxygen atom as the only hetero atom, condensed with other rings ortho- or peri-condensed with carbocyclic rings or ring systems
- C07D311/04—Benzo[b]pyrans, not hydrogenated in the carbocyclic ring
- C07D311/22—Benzo[b]pyrans, not hydrogenated in the carbocyclic ring with oxygen or sulfur atoms directly attached in position 4
- C07D311/26—Benzo[b]pyrans, not hydrogenated in the carbocyclic ring with oxygen or sulfur atoms directly attached in position 4 with aromatic rings attached in position 2 or 3
- C07D311/40—Separation, e.g. from natural material; Purification
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/50—Improvements relating to the production of bulk chemicals
- Y02P20/54—Improvements relating to the production of bulk chemicals using solvents, e.g. supercritical solvents or ionic liquids
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Pharmaceuticals Containing Other Organic And Inorganic Compounds (AREA)
- Medicines Containing Plant Substances (AREA)
Abstract
The invention discloses a method for extracting quercetin from plantain seeds, which belongs to the technical field of quercetin extraction and comprises the following steps: (1) coarsely pulverizing fresh semen plantaginis, then placing into sieve basket, and immersing into liquid nitrogen for treatment, repeating the above steps for 2-3 times; (2) drying the plantain seeds obtained in the step (1) at a low temperature, and crushing to obtain plantain seed powder; (3) extracting semen plantaginis powder by supercritical CO2 extraction; (4) and (3) allowing CO2 containing the extract to flow out of the extraction kettle, and allowing the extract to enter a separation kettle for reduced pressure separation to obtain the plantain seed quercetin. The method for extracting quercetin from semen plantaginis provided by the invention avoids considering the loss of quercetin in the semen plantaginis extraction process, and improves the quality and yield of quercetin extracted from semen plantaginis.
Description
Technical Field
The invention relates to a method for extracting quercetin from natural plants, in particular to a method for extracting quercetin from plantain seeds.
Background
Plantago asiatica L, Plantago asiatica, etc., biennial or perennial herbs,
china is cultivated in more provinces. It is originated from grassland, ditch, riverbank wetland, field, roadside or open area of village, and herba plantaginis is whole plant of Plantago asiatica and Plantago depressa of Plantaginaceae, and has sweet taste and cold property. Has expectorant, antitussive, and antiasthmatic effects. The plantain herb is a traditional Chinese medicine for promoting diuresis and excreting dampness, and mainly treats the following diseases: it is indicated for dysuria, stranguria with turbid discharge, edema, fullness and distention, summer-heat and dampness, dysentery, conjunctival congestion, nebula, phlegm-heat cough and asthma. The plantain leaves not only have obvious diuretic effect, but also have obvious effects of eliminating phlegm, resisting bacteria and reducing blood pressure. It can act on respiratory center and has strong antitussive effect. Can promote secretion of mucus in trachea and bronchus, and has expectorant effect.
The traditional quercetin extraction process mainly comprises a water distillation method, a solvent extraction method, supercritical fluid extraction, direct steam distillation and microwave-assisted extraction, and the ultrasonic extraction process and the semi-bionic extraction technology are less applied to the extraction research of essential oil in enterprises. The water distillation and solvent extraction methods inevitably cause changes in the components, thereby changing the overall flavor profile, and often lose top note, the product loses freshness, and contamination with solvent residues is difficult to avoid. And the CO2 fluid of the supercritical CO2 has a new separation technology with special solubility effect on organic matters. The technology has unique advantages for separating macromolecular, heat-sensitive or chemically unstable substances which are difficult to solve by the traditional separation method, so that the technology receives wide attention in the fields of food, spice, medicine, chemical industry and the like.
Disclosure of Invention
The invention aims to provide a method for extracting quercetin from semen plantaginis, which aims to solve the problems in the prior art and avoid the loss of effective components in the semen plantaginis treatment.
In order to achieve the above object, the present invention is implemented by the following technical solutions: a method for extracting quercetin from semen plantaginis comprises the following steps:
(1) coarsely pulverizing fresh semen plantaginis, soaking in water, placing into sieve basket, totally immersing in liquid nitrogen for 30-60min, lifting, placing at room temperature for 5-10min, totally immersing sieve basket in liquid nitrogen for 30-60min, and repeating for 2-3 times;
(2) drying the plantain seeds obtained in the step (1) at a low temperature, crushing, and sieving with a 5-30-mesh sieve to obtain plantain seed powder;
(3) mixing semen plantaginis powder and solvent, placing into an extraction kettle, introducing supercritical CO2 into the extraction kettle, controlling the temperature of the extraction kettle at 40-50 deg.C and the extraction pressure at 30-45 Mpa;
(4) and (3) allowing CO2 containing the extract to flow out of the extraction kettle, and allowing the extract to enter a separation kettle for reduced pressure separation to obtain the plantain seed quercetin.
By immersing the water-rich plantain seeds into low-temperature liquid nitrogen, water in cell sap is frozen, the volume is enlarged, cell walls are punctured, effective components in plantain seed cells are promoted to be separated out, and then the plantain seeds are dried under the low-temperature condition, so that the effective components in the plantain seeds are prevented from being lost. According to the invention, the low-temperature vacuum drying process comprises the following steps: alternately stacking folium Artemisiae Argyi in vacuum drying oven, controlling vacuum degree at 0.009-0.36Mpa, and vacuum drying at 40-52 deg.C.
Preferably, the plantain seeds are dried until the water content is below 5%.
according to the invention, in order to further separate out effective components in the plantain seeds, the plantain seed powder is fully mixed with 0.01-0.08 times of biological enzyme and stands for 30-60min before being implanted into an extraction kettle, and the cell walls of the plantain seeds are decomposed by the biological enzyme, preferably, the biological enzyme is at least one of β -glucosidase, pectinase and cellulase.
According to the present invention, in order to facilitate the subsequent removal of the solvent, the solvent of the present invention is a low boiling point solvent, and preferably, the solvent is at least one of acetone, ethanol, methanol and dichloromethane.
According to the invention, the pressure of the separation kettle is 7-9Mpa, and the temperature is 25-30 ℃.
Compared with the prior art, the method for extracting quercetin from semen plantaginis effectively avoids the loss of effective components in the semen plantaginis extraction process, and improves the quality and yield of quercetin extracted from semen plantaginis.
The specific implementation mode is as follows:
in order to make the technical means, the creation features, the achievement purposes and the effects of the invention easy to understand, the invention is further clarified with the specific embodiments.
Example 1:
a method for extracting quercetin from semen plantaginis comprises the following steps:
(1) coarsely pulverizing fresh semen plantaginis, soaking in water for 25min, placing into sieve basket, totally immersing in liquid nitrogen for 50min, lifting, placing at room temperature for 8min, totally immersing sieve basket in liquid nitrogen for 50min, and repeating the above steps for 3 times;
(2) drying the plantain seeds obtained in the step (1) at a low temperature, crushing, and sieving by a 20-mesh sieve to obtain plantain seed powder;
the low-temperature vacuum drying process comprises the following steps: staggered piling of semen plantaginis in a vacuum drying oven, controlling vacuum degree at 0.009Mpa and vacuum drying temperature at 40 deg.C, and oven drying semen plantaginis until water content is below 5%;
(3) mixing semen plantaginis powder with 0.05 times weight of beta-glucosidase, standing for 50min, mixing with acetone, placing into an extraction kettle, introducing supercritical CO2 into the extraction kettle, controlling the temperature of the extraction kettle at 45 deg.C and the extraction pressure at 40 Mpa;
(4) and allowing CO2 containing the extract to flow out of the extraction kettle, and separating under reduced pressure in a separation kettle at 28 deg.C under 8Mpa to obtain quercetin.
Example 2:
a method for extracting quercetin from semen plantaginis comprises the following steps:
(1) coarsely pulverizing fresh semen plantaginis, soaking in water for 20min, placing into sieve basket, totally immersing in liquid nitrogen for 30min, lifting, placing at room temperature for 5min, totally immersing sieve basket in liquid nitrogen for 30min, and repeating for 2 times;
(2) drying the plantain seeds obtained in the step (1) at a low temperature, crushing and sieving with a 5-mesh sieve to obtain plantain seed powder;
the low-temperature vacuum drying process comprises the following steps: staggered piling of semen plantaginis in a vacuum drying oven, controlling vacuum degree at 0.009Mpa and vacuum drying temperature at 40 deg.C, and oven drying semen plantaginis until water content is below 5%;
(3) mixing semen plantaginis powder with 0.01 times of pectinase, standing for 30min, mixing with ethanol, and placing into an extraction kettle, introducing supercritical CO2 into the extraction kettle, controlling the temperature of the extraction kettle at 40 deg.C and the extraction pressure at 30 Mpa;
(4) and allowing CO2 containing the extract to flow out of the extraction kettle, and separating under reduced pressure in a separation kettle at 20 deg.C under 5Mpa to obtain quercetin.
Example 3:
a method for extracting quercetin from semen plantaginis comprises the following steps:
(1) coarsely pulverizing fresh semen plantaginis, soaking in water for 30min, placing into sieve basket, totally immersing in liquid nitrogen for 60min, lifting, placing at room temperature for 10min, totally immersing sieve basket in liquid nitrogen for 60min, and repeating the steps for 3 times;
(2) drying the plantain seeds obtained in the step (1) at a low temperature, crushing, and sieving by a 30-mesh sieve to obtain plantain seed powder;
the low-temperature vacuum drying process comprises the following steps: staggered piling of semen plantaginis in a vacuum drying oven, controlling vacuum degree at 0.009Mpa and vacuum drying temperature at 40 deg.C, and oven drying semen plantaginis until water content is below 5%;
(3) mixing semen plantaginis powder with 0.08 times weight of cellulase, stirring thoroughly, standing for 60min, mixing with acetone, placing into an extraction kettle, introducing supercritical CO2 into the extraction kettle, controlling the temperature of the extraction kettle at 50 deg.C and the extraction pressure at 45 Mpa;
(4) and allowing CO2 containing the extract to flow out of the extraction kettle, and separating under reduced pressure in a separation kettle at 30 deg.C under 10Mpa to obtain quercetin.
The foregoing shows and describes the general principles, essential features, and inventive features of this invention. The present invention is not limited to the above-described embodiments, and the above-described embodiments and the description are only for illustrating the principle of the present invention, and various changes and modifications may be made without departing from the spirit and scope of the present invention, and these changes and modifications are all within the scope of the present invention.
Claims (6)
1. A method for extracting quercetin from semen plantaginis is characterized by comprising the following steps:
(1) coarsely pulverizing fresh semen plantaginis, soaking in water, placing into sieve basket, totally immersing in liquid nitrogen for 30-60min, lifting, placing at room temperature for 5-10min, totally immersing sieve basket in liquid nitrogen for 30-60min, and repeating for 2-3 times;
(2) drying the plantain seeds obtained in the step (1) at a low temperature, crushing, and sieving with a 5-30-mesh sieve to obtain plantain seed powder;
(3) mixing semen plantaginis powder and solvent, placing into an extraction kettle, introducing supercritical CO2 into the extraction kettle, controlling the temperature of the extraction kettle at 40-50 deg.C and the extraction pressure at 30-45 Mpa;
(4) and allowing CO2 containing the extract to flow out of the extraction kettle, and allowing the extract to enter a separation kettle for reduced pressure separation to obtain quercetin.
2. the method for extracting quercetin from semen plantaginis according to claim 1, wherein in the step (3), semen plantaginis powder is fully and uniformly mixed with 0.01-0.08 times of weight of biological enzyme before being placed in an extraction kettle and is kept still for 30-60min, wherein the biological enzyme is one of β -glucosidase, pectinase and cellulase.
3. The method of extracting quercetin from psyllium seed according to claim 1, wherein: in the step (2), the plantain seeds are dried in vacuum at low temperature, and the process comprises the following steps: staggered-piling semen plantaginis in vacuum drying oven, controlling vacuum degree at 0.009-0.36Mpa, and vacuum drying at 40-52 deg.C.
4. The method of extracting quercetin from psyllium seed according to claim 1, wherein: in the step (2), the plantain seeds are dried until the water content is below 5%.
5. The method of extracting quercetin from psyllium seed according to claim 1, wherein: the solvent is a low-boiling point solvent, and preferably, the solvent is at least one of acetone, ethanol, diethyl ether, methanol and dichloromethane.
6. The method of extracting quercetin from psyllium seed according to claim 1, wherein: in the step (4), the pressure of the separation kettle is 7-9Mpa, and the temperature is 25-30 ℃.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811419102.1A CN111217784A (en) | 2018-11-26 | 2018-11-26 | Method for extracting quercetin from plantain seeds |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811419102.1A CN111217784A (en) | 2018-11-26 | 2018-11-26 | Method for extracting quercetin from plantain seeds |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN111217784A true CN111217784A (en) | 2020-06-02 |
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201811419102.1A Withdrawn CN111217784A (en) | 2018-11-26 | 2018-11-26 | Method for extracting quercetin from plantain seeds |
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| Country | Link |
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| CN (1) | CN111217784A (en) |
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2018
- 2018-11-26 CN CN201811419102.1A patent/CN111217784A/en not_active Withdrawn
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Application publication date: 20200602 |
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| WW01 | Invention patent application withdrawn after publication |