CN110551005A - Preparation method of magnolol - Google Patents
Preparation method of magnolol Download PDFInfo
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- CN110551005A CN110551005A CN201810536730.1A CN201810536730A CN110551005A CN 110551005 A CN110551005 A CN 110551005A CN 201810536730 A CN201810536730 A CN 201810536730A CN 110551005 A CN110551005 A CN 110551005A
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- concentrating
- magnolol
- extracting
- under reduced
- reduced pressure
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C37/00—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom of a six-membered aromatic ring
- C07C37/004—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom of a six-membered aromatic ring by obtaining phenols from plant material or from animal material
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Botany (AREA)
- Medicines Containing Plant Substances (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention relates to a preparation method of magnolol, which comprises the processing steps of a, drying and crushing magnolia officinalis, sieving with a 20-mesh sieve, b, adding absolute ethyl alcohol with the mass of 5 ~ 10 times of that of the raw material, soaking for 1h, placing in an ultrasonic-microwave extraction device, setting ultrasonic waves of 280W, extracting for 1 ~ 4h with the microwave power of 100 ~ 300W, c, centrifuging, concentrating the obtained supernatant under reduced pressure until no alcohol smell exists, adjusting the pH value to 8 ~ 9 with ammonia water, d, concentrating the eluate under reduced pressure, extracting with an organic solvent for 3 times, and concentrating and drying the obtained extract in vacuum to obtain magnolol.
Description
Technical Field
The invention relates to a preparation method of magnolol, in particular to a method for extracting magnolol by using ultrasonic-microwave.
Background
The cortex Magnolia officinalis is dry bark, root bark or branch bark of Magnolia officinalis (Magnolia officinalis Rend et Wils) of Magnoliaceae, has warm and bitter taste, is nontoxic, and can enter spleen, stomach and large intestine channels, warm middle-jiao and lower qi, eliminate dampness and eliminate phlegm. The magnolia officinalis has medicinal history of more than two thousand years, can be used for treating diseases of a plurality of systems and organs, and a plurality of Chinese medicinal proved formulas in China such as magnolia officinalis three-material decoction, Pingwei powder, Dachengqi decoction, Siqi decoction and gardenia magnolia officinalis decoction all contain crude drug magnolia officinalis; in one part of the 2005 edition of Chinese pharmacopoeia, more than 20 commonly used Chinese patent medicines including Huoxiang Zhengqi liquid, Xiangsha Yangwei Wan, Kaixiong Shuqi Wan, chaihu Shugan Wan, etc. contain Magnolia officinalis as the main raw material. Modern pharmacological studies show that the magnolia officinalis has the effects of resisting bacteria, viruses and allergy, influencing gastrointestinal activities, relaxing muscles, inhibiting the center of the stomach and the intestine and the like. Magnolol and honokiol are main phenolic compounds in the magnolia officinalis medicinal material and main substances with medicinal effects in the magnolia officinalis medicinal material, and the content of the two phenols is a mark for evaluating the quality of the magnolia officinalis medicinal material.
at present, a plurality of patents and documents are provided for extracting magnolol, and a plurality of defects exist in the methods of mainly using a solvent extraction method, a supercritical fluid extraction method, an acid water percolation method and the like. The supercritical extraction method has the defects of high equipment cost and unsuitability for industrial production; the acid water percolation method is mostly adopted for extraction in industry at present, and the defects of the method are that the operation is complicated, the extraction rate is low, and the waste liquid amount is large.
disclosure of Invention
The invention aims to provide a method for extracting magnolol, which is simple in process, easy to operate, rapid and efficient, aiming at the defects of the prior art.
The invention comprises the following steps:
a. Drying and crushing the mangnolia officinalis, and sieving the mangnolia officinalis with a 20-mesh sieve;
b. Adding absolute ethyl alcohol with the mass 5 ~ 10 times of that of the raw material, soaking for 1h, placing in an ultrasonic-microwave extraction device, setting ultrasonic waves at 280W and microwave power at 100 ~ 300W, and extracting for 1 ~ 4 h;
c. centrifuging, concentrating the obtained supernatant under reduced pressure until no alcohol smell exists, and adjusting the pH value to 8 ~ 9 with ammonia water;
d. concentrating the eluate under reduced pressure, extracting with organic solvent for 3 times, concentrating the obtained extractive solution, and vacuum drying to obtain magnolol.
The microwave power in the step b is 100 ~ 300W, and the extraction time is 1 ~ 4 h.
And d, the organic solvent is petroleum ether.
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:
Drying and crushing the mangnolia officinalis, and sieving the mangnolia officinalis with a 20-mesh sieve; adding absolute ethyl alcohol with the mass 5 times of that of the raw materials, soaking for 1 hour, placing in an ultrasonic-microwave extraction device, setting ultrasonic waves at 280W and microwave power at 100W, and extracting for 1 hour; centrifuging, concentrating the obtained supernatant under reduced pressure until no alcohol smell exists, and adjusting the pH value to 8 with ammonia water; concentrating the eluate under reduced pressure, extracting with organic solvent petroleum ether for 3 times, concentrating the obtained extractive solution, and vacuum drying to obtain magnolol.
Example 2:
Drying and crushing the mangnolia officinalis, and sieving the mangnolia officinalis with a 20-mesh sieve; adding absolute ethyl alcohol with the mass 6 times of that of the raw materials, soaking for 1h, placing in an ultrasonic-microwave extraction device, setting ultrasonic waves at 280W and microwave power at 200W, and extracting for 2 h; centrifuging, concentrating the obtained supernatant under reduced pressure until no alcohol smell exists, and adjusting the pH value to 9 with ammonia water; concentrating the eluate under reduced pressure, extracting with organic solvent petroleum ether for 3 times, concentrating the obtained extractive solution, and vacuum drying to obtain magnolol.
Example 3:
Drying and crushing the mangnolia officinalis, and sieving the mangnolia officinalis with a 20-mesh sieve; adding absolute ethyl alcohol with the weight 10 times of that of the raw materials, soaking for 1h, placing in an ultrasonic-microwave extraction device, setting ultrasonic waves at 280W and microwave power at 300W, and extracting for 4 h; centrifuging, concentrating the obtained supernatant under reduced pressure until no alcohol smell exists, and adjusting the pH value to 8 with ammonia water; concentrating the eluate under reduced pressure, extracting with organic solvent petroleum ether for 3 times, concentrating the obtained extractive solution, and vacuum drying to obtain magnolol.
Claims (3)
1. A preparation method of magnolol is characterized by comprising the following steps:
a. drying and crushing the mangnolia officinalis, and sieving the mangnolia officinalis with a 20-mesh sieve;
b. adding absolute ethyl alcohol with the mass 5 ~ 10 times of that of the raw material, soaking for 1h, placing in an ultrasonic-microwave extraction device, setting ultrasonic waves at 280W and microwave power at 100 ~ 300W, and extracting for 1 ~ 4 h;
c. Centrifuging, concentrating the obtained supernatant under reduced pressure until no alcohol smell exists, and adjusting the pH value to 8 ~ 9 with ammonia water;
d. concentrating the eluate under reduced pressure, extracting with organic solvent for 3 times, concentrating the obtained extractive solution, and vacuum drying to obtain magnolol.
2. The method of claim 1, wherein the microwave power in step b is 100 ~ 300W, and the extraction time is 1 ~ 4 h.
3. The method of claim 1, wherein the organic solvent of step d is petroleum ether.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810536730.1A CN110551005A (en) | 2018-05-30 | 2018-05-30 | Preparation method of magnolol |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810536730.1A CN110551005A (en) | 2018-05-30 | 2018-05-30 | Preparation method of magnolol |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN110551005A true CN110551005A (en) | 2019-12-10 |
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201810536730.1A Pending CN110551005A (en) | 2018-05-30 | 2018-05-30 | Preparation method of magnolol |
Country Status (1)
| Country | Link |
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| CN (1) | CN110551005A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113713425A (en) * | 2021-09-07 | 2021-11-30 | 山东一方制药有限公司 | Process method for extracting magnolia officinalis by utilizing continuous dynamic countercurrent |
-
2018
- 2018-05-30 CN CN201810536730.1A patent/CN110551005A/en active Pending
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113713425A (en) * | 2021-09-07 | 2021-11-30 | 山东一方制药有限公司 | Process method for extracting magnolia officinalis by utilizing continuous dynamic countercurrent |
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Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20191210 |
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| WD01 | Invention patent application deemed withdrawn after publication |