CN111187307A - Method for extracting aucubin from eucommia ulmoides bark - Google Patents
Method for extracting aucubin from eucommia ulmoides bark Download PDFInfo
- Publication number
- CN111187307A CN111187307A CN201811355902.1A CN201811355902A CN111187307A CN 111187307 A CN111187307 A CN 111187307A CN 201811355902 A CN201811355902 A CN 201811355902A CN 111187307 A CN111187307 A CN 111187307A
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- Prior art keywords
- aucubin
- bark
- eucommia
- eucommia ulmoides
- extraction
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07H—SUGARS; DERIVATIVES THEREOF; NUCLEOSIDES; NUCLEOTIDES; NUCLEIC ACIDS
- C07H1/00—Processes for the preparation of sugar derivatives
- C07H1/06—Separation; Purification
- C07H1/08—Separation; Purification from natural products
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07H—SUGARS; DERIVATIVES THEREOF; NUCLEOSIDES; NUCLEOTIDES; NUCLEIC ACIDS
- C07H17/00—Compounds containing heterocyclic radicals directly attached to hetero atoms of saccharide radicals
- C07H17/04—Heterocyclic radicals containing only oxygen as ring hetero atoms
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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)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Biochemistry (AREA)
- Biotechnology (AREA)
- General Health & Medical Sciences (AREA)
- Genetics & Genomics (AREA)
- Molecular Biology (AREA)
- Medicines Containing Plant Substances (AREA)
- Coloring Foods And Improving Nutritive Qualities (AREA)
Abstract
The invention discloses a method for extracting aucubin from eucommia ulmoides bark, which belongs to the technical field of aucubin extraction and comprises the following steps: (1) coarsely pulverizing fresh cortex Eucommiae, placing into sieve basket, immersing in liquid nitrogen, and repeating for 2-3 times; (2) drying and crushing the eucommia bark in the step (1) at a low temperature to obtain eucommia bark powder; (3) extracting cortex Eucommiae powder by supercritical CO2 extraction method; (4) CO2 containing the extract flows out of the extraction kettle, enters a separation kettle for decompression separation to obtain the eucommia ulmoides oliv aucubin. The method for extracting aucubin from eucommia ulmoides oliver provided by the invention avoids considering the loss of aucubin in the extraction process of eucommia ulmoides oliver, and improves the quality and yield of extracting aucubin from eucommia ulmoides oliver.
Description
Technical Field
The invention relates to a method for extracting aucubin from natural plants, in particular to a method for extracting aucubin from eucommia ulmoides bark.
Background
Eucommia ulmoides, also known as Bakelite, is a plant of the family Eucommiaceae. The eucommia bark contains few free amino acids, but contains a small amount of protein which is complete protein similar to most foods, can hydrolyze and detect 8 kinds of amino acids necessary for human bodies, and contains 15 kinds of mineral elements such as trace elements of zinc, copper, iron and the like, and trace elements of calcium, phosphorus, potassium, magnesium and the like. Medicinal eucommia bark, namely dried bark of eucommia bark which is a plant of eucommia family, is a rare and nourishing medicinal material in China. It is sweet in taste and warm in nature. Has effects in tonifying liver and kidney, strengthening muscle and bone, regulating Chong and ren meridians, and preventing miscarriage. Can be used for treating lumbago, leg pain, soreness, weakness, and asthenia due to kidney yang deficiency, and symptoms such as hypochondriac instability, and scrotum pruritus due to liver qi deficiency. It is listed as the superior in Shen nong Ben Cao Jing. Aucubin is one of effective active ingredients in Eucommiae cortex, belongs to iridoid, and has antiinflammatory, antibacterial, damp-heat clearing away, urination promoting, and blood pressure increasing effects.
The traditional extraction process of aucubin mainly comprises a water distillation method, a solvent extraction method, a supercritical fluid extraction method, direct steam distillation and a microwave-assisted extraction process, and the ultrasonic extraction process and the semi-bionic extraction technology are less applied to the extraction research of essential oil of 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
In view of the problems in the prior art, the invention aims to provide a method for extracting aucubin from eucommia ulmoides bark, which avoids the loss of effective components in the treatment of eucommia ulmoides bark.
In order to achieve the above object, the present invention is implemented by the following technical solutions: a method for extracting aucubin from eucommia bark comprises the following steps:
(1) coarsely crushing fresh eucommia bark, soaking in water, then putting into a sieve basket, totally immersing into liquid nitrogen for 30-60min, then lifting, placing at room temperature for 5-10min, totally immersing the sieve basket into the liquid nitrogen for 30-60min, and repeating the steps for 2-3 times;
(2) drying the eucommia bark in the step (1) at a low temperature, crushing, and sieving with a 5-30-mesh sieve to obtain eucommia bark powder;
(3) mixing cortex Eucommiae powder with 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) CO2 containing the extract flows out of the extraction kettle, enters a separation kettle for decompression separation to obtain the eucommia ulmoides oliv aucubin.
Through submerging the cortex eucommiae of rich water in microthermal liquid nitrogen, water in the cell sap freezes, and the cell wall is punctureed to the grow in volume, impels the active ingredient in the cortex eucommiae cell to separate out, then dries under microthermal condition, has ensured that active ingredient can not run off in the cortex eucommiae. 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 eucommia bark is dried until the water content is below 5 percent.
According to the invention, in order to further separate out effective components in the eucommia bark, before the eucommia bark powder is implanted into an extraction kettle, the eucommia bark powder is fully mixed with 0.01-0.08 times of biological enzyme and stands for 30-60min, and the cell wall of the eucommia bark is 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 aucubin from eucommia ulmoides oliver provided by the invention effectively avoids the loss of effective components in the extraction process of eucommia ulmoides oliver, and improves the quality and yield of aucubin extracted from eucommia ulmoides oliver.
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 aucubin from eucommia bark comprises the following steps:
(1) coarsely crushing fresh cortex Eucommiae, soaking in water for 25min, placing into screen basket, totally soaking in liquid nitrogen for 50min, lifting, placing at room temperature for 8min, totally soaking screen basket in liquid nitrogen for 50min, and repeating the steps for 3 times;
(2) drying the eucommia bark in the step (1) at a low temperature, crushing, and sieving with a 20-mesh sieve to obtain eucommia bark powder;
the low-temperature vacuum drying process comprises the following steps: alternately stacking cortex Eucommiae in a vacuum drying oven at vacuum degree of 0.009Mpa and vacuum drying temperature of 40 deg.C until water content is below 5%;
(3) mixing cortex Eucommiae powder with β -glucosidase 0.05 times of weight, 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 the CO2 containing the extract to flow out of the extraction kettle, and allowing the extract to enter a separation kettle for reduced pressure separation, wherein the pressure of the separation kettle is 8Mpa, and the temperature is 28 ℃, so as to obtain aucubin.
Example 2:
a method for extracting aucubin from eucommia bark comprises the following steps:
(1) coarsely crushing fresh cortex Eucommiae, soaking in water for 20min, placing into screen basket, totally soaking in liquid nitrogen for 30min, lifting, placing at room temperature for 5min, totally soaking screen basket in liquid nitrogen for 30min, and repeating the steps for 2 times;
(2) drying the eucommia bark in the step (1) at a low temperature, crushing, and sieving with a 5-mesh sieve to obtain eucommia bark powder;
the low-temperature vacuum drying process comprises the following steps: alternately stacking cortex Eucommiae in a vacuum drying oven at vacuum degree of 0.009Mpa and vacuum drying temperature of 40 deg.C until water content is below 5%;
(3) mixing cortex Eucommiae 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 aucubin.
Example 3:
a method for extracting aucubin from eucommia bark comprises the following steps:
(1) coarsely crushing fresh cortex Eucommiae, soaking in water for 30min, placing into screen basket, totally soaking in liquid nitrogen for 60min, lifting, placing at room temperature for 10min, totally soaking screen basket in liquid nitrogen for 60min, and repeating the steps for 3 times;
(2) drying the eucommia bark in the step (1) at a low temperature, crushing, and sieving with a 30-mesh sieve to obtain eucommia bark powder;
the low-temperature vacuum drying process comprises the following steps: alternately stacking cortex Eucommiae in a vacuum drying oven at vacuum degree of 0.009Mpa and vacuum drying temperature of 40 deg.C until water content is below 5%;
(3) mixing cortex Eucommiae powder with 0.08 times of cellulase, 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 aucubin.
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 aucubin from eucommia ulmoides bark is characterized by comprising the following steps:
(1) coarsely crushing fresh eucommia bark, soaking in water, then putting into a sieve basket, totally immersing into liquid nitrogen for 30-60min, then lifting, placing at room temperature for 5-10min, totally immersing the sieve basket into the liquid nitrogen for 30-60min, and repeating the steps for 2-3 times;
(2) drying the eucommia bark in the step (1) at a low temperature, crushing, and sieving with a 5-30-mesh sieve to obtain eucommia bark powder;
(3) mixing cortex Eucommiae powder with 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 separating in a separation kettle under reduced pressure to obtain aucubin.
2. The method for extracting aucubin from eucommia ulmoides oliver as claimed in claim 1, wherein in step (3), the eucommia ulmoides oliver powder is mixed with 0.01-0.08 times weight of biological enzyme (β -glucosidase, pectinase and cellulase) before being placed in the extraction kettle, and is left for 30-60 min.
3. The method of claim 1, wherein the aucubin is extracted from eucommia ulmoides oliv nakai bark: in the step (2), the eucommia bark is dried in vacuum at low temperature, and the process comprises the following steps: alternately stacking cortex Eucommiae in a vacuum drying oven at vacuum degree of 0.009-0.36Mpa and vacuum drying temperature of 40-52 deg.C.
4. The method of claim 1, wherein the aucubin is extracted from eucommia ulmoides oliv nakai bark: in the step (2), the eucommia ulmoides bark is dried until the water content is below 5%.
5. The method of claim 1, wherein the aucubin is extracted from eucommia ulmoides oliv nakai bark: 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 claim 1, wherein the aucubin is extracted from eucommia ulmoides oliv nakai bark: 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 |
|---|---|---|---|
| CN201811355902.1A CN111187307A (en) | 2018-11-15 | 2018-11-15 | Method for extracting aucubin from eucommia ulmoides bark |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811355902.1A CN111187307A (en) | 2018-11-15 | 2018-11-15 | Method for extracting aucubin from eucommia ulmoides bark |
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| Publication Number | Publication Date |
|---|---|
| CN111187307A true CN111187307A (en) | 2020-05-22 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201811355902.1A Withdrawn CN111187307A (en) | 2018-11-15 | 2018-11-15 | Method for extracting aucubin from eucommia ulmoides bark |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113209153A (en) * | 2021-04-30 | 2021-08-06 | 江西普正制药股份有限公司 | Eucommia ulmoides composition, preparation method and application thereof |
-
2018
- 2018-11-15 CN CN201811355902.1A patent/CN111187307A/en not_active Withdrawn
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113209153A (en) * | 2021-04-30 | 2021-08-06 | 江西普正制药股份有限公司 | Eucommia ulmoides composition, preparation method and application thereof |
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| PB01 | Publication | ||
| PB01 | Publication | ||
| WW01 | Invention patent application withdrawn after publication |
Application publication date: 20200522 |
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| WW01 | Invention patent application withdrawn after publication |