CN110551167A - Method for preparing astragaloside - Google Patents
Method for preparing astragaloside Download PDFInfo
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- CN110551167A CN110551167A CN201810536969.9A CN201810536969A CN110551167A CN 110551167 A CN110551167 A CN 110551167A CN 201810536969 A CN201810536969 A CN 201810536969A CN 110551167 A CN110551167 A CN 110551167A
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- astragaloside
- supernatant
- astragalus
- centrifuging
- 10min
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07J—STEROIDS
- C07J53/00—Steroids in which the cyclopenta(a)hydrophenanthrene skeleton has been modified by condensation with a carbocyclic rings or by formation of an additional ring by means of a direct link between two ring carbon atoms, including carboxyclic rings fused to the cyclopenta(a)hydrophenanthrene skeleton are included in this class
- C07J53/002—Carbocyclic rings fused
- C07J53/004—3 membered carbocyclic rings
Abstract
The invention relates to a preparation method of astragaloside, in particular to a method for extracting astragaloside by adopting an enzyme method-ultrasonic wall breaking method, which comprises the processing steps of preparing astragalus, crushing and grinding the astragalus into powder, adding a citric acid-disodium hydrogen phosphate buffer solution with a pH value of 4.5 according to a feed-liquid ratio of 1:5, uniformly mixing, adding 17% of cellulase according to the mass, carrying out enzymolysis for 1h at 55 ℃, centrifuging for 10min at 4000r/min, collecting a supernatant, taking a proper amount of enzyme method wall breaking precipitate, respectively adding warm water, 50% ~ 60% of absolute ethyl alcohol and 0.05mol/L of citric acid-disodium hydrogen phosphate buffer solution with a pH value of 3.7 according to a feed-liquid ratio of 1:5, extracting for 30 ~ 40min, carrying out ultrasonic auxiliary extraction under the same condition, centrifuging for 10min at 4000r/min after the extraction is finished, taking the supernatant, combining the two times of supernatant, and drying at 60 ℃ to obtain the astragaloside.
Description
Technical Field
The invention relates to a preparation method of astragaloside, belonging to the field of extraction of effective components of traditional Chinese medicines.
background
Astragalus membranaceus is a pure natural product which is frequently eaten by people, and people have a smooth running of 'frequently drinking astragalus soup, preventing diseases and protecting health', which means that astragalus membranaceus is frequently used for decocting or soaking in water to replace tea for drinking, and the astragalus membranaceus has good disease prevention and health care effects. Radix astragali and ginseng both belong to good qi-tonifying drugs, and ginseng is mainly used for tonifying primordial qi and restoring yang from collapse, and is commonly used for treating acute diseases such as collapse, shock and the like with good effect. While Huang Qi is mainly tonifying deficiency, it is commonly indicated for chronic weakness, low speech and weak pulse. Some people are easy to catch cold when they meet weather change, the traditional Chinese medicine is called as 'exterior insecurity', astragalus can be used for strengthening exterior, and frequent taking of astragalus can avoid frequent cold. Modern medical research shows that astragalus has the functions of enhancing the immunity of organisms, protecting the liver, promoting urination, resisting aging, resisting stress, reducing blood pressure and resisting a wide range of bacteria. Can eliminate albuminuria caused by experimental nephritis, enhance myocardial contraction force, and regulate blood sugar content. Radix astragali can not only dilate coronary artery, improve myocardial blood supply, and enhance immunity, but also delay cell aging process. The astragalus root is convenient to eat and can be used for decocting soup, decocting paste, soaking wine, adding into dishes and the like.
The main effective components of astragalus polysaccharide are polysaccharide and astragaloside. The astragalosides include astragaloside I, astragaloside II and astragaloside IV. Wherein the bioactive agent is astragaloside IV, i.e. astragaloside IV. The astragaloside IV not only has the function of astragalus polysaccharide, but also has incomparable function of the astragalus polysaccharide, the drug effect strength of the astragaloside IV is more than 2 times of that of the conventional astragalus polysaccharide, and the antiviral effect of the astragaloside IV is more than 30 times of that of the astragalus polysaccharide. Because of the low content and good effect, the super astragalus polysaccharide is called.
At present, acid hydrolysis method and pre-fermentation method are mostly adopted for extracting astragaloside IV. The acid hydrolysis method has large acid consumption, and a large amount of organic matter degradation byproducts are generated by acid, so that the sewage discharge amount is large, the environmental pollution is serious, and the industrialized development of the astragaloside IV is limited. The method for extracting astragaloside IV by adopting a pre-fermentation method is long in time consumption and unstable in product quality.
The enzymatic method-ultrasonic wall breaking extraction refers to the wall breaking treatment of plant cells by cellulase. To extract the effective components in the tissue. The effective components in the plant are extracted by an enzyme method, after the wall breaking treatment is carried out on the plant, different tissues and parts of the same plant can be highly and uniformly mixed due to cell breakage, the uniformity of the material basis of products in the plant is realized, a high-temperature solvent extraction process is not needed, the links of effective loss are reduced, and the total components of the original plant are retained to the maximum extent.
and the cavitation effect and the mechanical effect of the ultrasonic wave are combined, so that the effective components in the cells are released to be directly contacted with the solvent and dissolved in the solvent, and the extraction rate of the effective components is improved.
Disclosure of Invention
The invention aims at overcoming the defects of the prior art and aims at providing a method for preparing astragaloside IV, which has high efficiency and selectivity, is simple and convenient to operate, has high yield and few byproducts and can be industrially realized.
The technical scheme of the invention is carried out according to the following steps:
a. Preparing astragalus, crushing and grinding the astragalus into powder, adding a citric acid-disodium hydrogen phosphate buffer solution with the pH value of 4.5 according to the material-liquid ratio of 1:5, uniformly mixing, adding 17% of cellulase according to the mass, performing enzymolysis at 55 ℃ for 1h, centrifuging at 4000r/min for 10min, and collecting a supernatant.
b. Taking a proper amount of enzyme-method wall-broken precipitate, adding warm water, 50% ~ 60% absolute ethanol and 0.05mol/L citric acid-disodium hydrogen phosphate buffer solution with the pH value of 3.7 into the mixture according to the material-liquid ratio of 1:5, extracting for 30 ~ 40min, and performing ultrasonic-assisted extraction under the same conditions.
c. After extraction, centrifuging at 4000r/min for 10min, collecting supernatant, mixing the two supernatants, and drying at 60 deg.C to obtain astragaloside IV.
2. the power of the centrifugal machine in the step a is 900W, and the rotating speed is 1000 ~ 20000 r/min.
3. the ultrasonic extraction conditions in the step b are that the frequency is 30KHz, and the ultrasonic temperature is 30 ~ 40 ℃.
4. The power of the centrifugal machine in the step c is 900W, and the rotating speed is 1000 ~ 20000 r/min.
The invention has the advantages that:
1. The invention adopts plant cellulase method to treat raw materials, realizes the wall breaking of plants, fully dissolves out the effective components, and avoids heating, thereby effectively avoiding the damage of astragaloside IV components.
2. The method for extracting the astragaloside IV by adopting the enzyme method-ultrasonic wall-breaking method has the advantages of high efficiency, higher content of effective components in the solution and stronger oxidation resistance.
The present invention will be further described with reference to specific embodiments, but the scope of the invention as claimed is not limited to the following embodiments.
The specific implementation mode is as follows:
Example 1:
Preparing astragalus membranaceus, crushing and grinding the astragalus membranaceus into powder, adding a citric acid-disodium hydrogen phosphate buffer solution with a pH value of 4.5 according to a material-liquid ratio of 1:5, uniformly mixing, adding 17% of cellulase according to the mass, carrying out enzymolysis for 1h at 55 ℃, centrifuging for 10min at 4000r/min, collecting a supernatant, taking an appropriate amount of enzyme-method wall-broken precipitate, adding warm water (30 ℃), 50% of absolute ethyl alcohol and a citric acid-disodium hydrogen phosphate buffer solution with a LPH value of 3.7 of 0.05mol/LPH according to the material-liquid ratio of 1:5 respectively, extracting for 30min, placing the materials in a 30KHz ultrasonic device for extraction under the same conditions, centrifuging for 10min at 4000r/min after extraction is finished, taking the supernatant, combining the supernatants, drying at 60 ℃ to obtain astragaloside, and detecting that the content of the astragaloside is 99.4%.
example 2:
preparing astragalus membranaceus, crushing and grinding the astragalus membranaceus into powder, adding a citric acid-disodium hydrogen phosphate buffer solution with a pH value of 4.5 according to a material-liquid ratio of 1:5, uniformly mixing, adding 17% of cellulase according to the mass, carrying out enzymolysis for 1h at 55 ℃, centrifuging for 10min at 4000r/min, collecting a supernatant, taking an appropriate amount of enzyme-method wall-broken precipitate, adding warm water (45 ℃), 55% of absolute ethyl alcohol and a citric acid-disodium hydrogen phosphate buffer solution with a LPH value of 3.7 of 0.05mol/LPH according to the material-liquid ratio of 1:5 respectively, extracting for 35min, placing the materials in a 30KHz ultrasonic device for extraction under the same conditions, centrifuging for 10min at 4000r/min after extraction is finished, taking the supernatant, combining the supernatants, drying at 60 ℃ to obtain astragaloside, and detecting that the content of the astragaloside is 99.6%.
Example 3:
Preparing astragalus membranaceus, crushing and grinding the astragalus membranaceus into powder, adding a citric acid-disodium hydrogen phosphate buffer solution with a pH value of 4.5 according to a material-liquid ratio of 1:5, uniformly mixing, adding 17% of cellulase according to the mass, carrying out enzymolysis for 1h at 55 ℃, centrifuging for 10min at 4000r/min, collecting a supernatant, taking an appropriate amount of enzyme-method wall-broken precipitate, adding warm water (50 ℃), 60% of absolute ethyl alcohol and a citric acid-disodium hydrogen phosphate buffer solution with a LPH value of 3.7 of 0.05mol/LPH according to the material-liquid ratio of 1:5 respectively, extracting for 40min, placing the materials in a 30KHz ultrasonic device for extraction under the same conditions, centrifuging for 10min at 4000r/min after extraction is finished, taking the supernatant, combining the supernatants, drying at 60 ℃ to obtain astragaloside, and detecting that the content of the astragaloside is 99.8%.
Claims (4)
1. A preparation method of astragaloside is characterized in that:
a. Preparing astragalus, crushing and grinding the astragalus into powder, adding a citric acid-disodium hydrogen phosphate buffer solution with the pH value of 4.5 according to the material-liquid ratio of 1:5, uniformly mixing, adding 17% of cellulase according to the mass, performing enzymolysis at 55 ℃ for 1h, centrifuging at 4000r/min for 10min, and collecting a supernatant.
b. Taking a proper amount of enzyme-method wall-broken precipitate, adding warm water, 50% ~ 60% absolute ethanol and 0.05mol/L citric acid-disodium hydrogen phosphate buffer solution with the pH value of 3.7 into the mixture according to the material-liquid ratio of 1:5, extracting for 30 ~ 40min, and performing ultrasonic-assisted extraction under the same conditions.
c. After extraction, centrifuging at 4000r/min for 10min, collecting supernatant, mixing the two supernatants, and drying at 60 deg.C to obtain scutellarin astragaloside IV.
2. The method for preparing astragaloside IV according to claim 1, wherein the centrifuge power in step a is 900W, and the rotation speed is 1000 ~ 20000 r/min.
3. the method for preparing astragaloside IV according to claim 1, wherein the ultrasonic extraction conditions in step b are 30KHz in frequency and 30 ~ 40 ℃ in ultrasonic temperature.
4. The method for preparing astragaloside IV according to claim 1, wherein the centrifuge power in step c is 900W, and the rotation speed is 1000 ~ 20000 r/min.
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Cited By (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN111671790A (en) * | 2020-07-10 | 2020-09-18 | 武倩 | Chinese herbal medicine micro-molecule fermentation extraction process |
CN112741237A (en) * | 2021-01-21 | 2021-05-04 | 甘肃陇萃堂营养保健食品股份有限公司 | Concentrated fruit juice capable of keeping stable content of astragaloside and preparation method thereof |
US20220024969A1 (en) * | 2020-07-21 | 2022-01-27 | Shanxi University | Method for extracting astragaloside iv from fresh radix astragali |
-
2018
- 2018-05-30 CN CN201810536969.9A patent/CN110551167A/en active Pending
Cited By (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN111671790A (en) * | 2020-07-10 | 2020-09-18 | 武倩 | Chinese herbal medicine micro-molecule fermentation extraction process |
US20220024969A1 (en) * | 2020-07-21 | 2022-01-27 | Shanxi University | Method for extracting astragaloside iv from fresh radix astragali |
CN112741237A (en) * | 2021-01-21 | 2021-05-04 | 甘肃陇萃堂营养保健食品股份有限公司 | Concentrated fruit juice capable of keeping stable content of astragaloside and preparation method thereof |
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Application publication date: 20191210 |