CN106831738B - Method for extracting and separating mangiferin from mango leaves - Google Patents
Method for extracting and separating mangiferin from mango leaves Download PDFInfo
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- CN106831738B CN106831738B CN201710057903.7A CN201710057903A CN106831738B CN 106831738 B CN106831738 B CN 106831738B CN 201710057903 A CN201710057903 A CN 201710057903A CN 106831738 B CN106831738 B CN 106831738B
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- C07D407/00—Heterocyclic compounds containing two or more hetero rings, at least one ring having oxygen atoms as the only ring hetero atoms, not provided for by group C07D405/00
- C07D407/02—Heterocyclic compounds containing two or more hetero rings, at least one ring having oxygen atoms as the only ring hetero atoms, not provided for by group C07D405/00 containing two hetero rings
- C07D407/04—Heterocyclic compounds containing two or more hetero rings, at least one ring having oxygen atoms as the only ring hetero atoms, not provided for by group C07D405/00 containing two hetero rings directly linked by a ring-member-to-ring-member bond
Abstract
The invention belongs to the field of plant extraction, and particularly relates to a method for extracting and separating mangiferin from mango leaves. The technical problem solved by the invention is to provide a brand-new method for extracting and separating mangiferin from mango leaves, which is simple and easy to operate and can obtain mangiferin with higher purity. The extraction method comprises the following steps of A, preparing raw materials; B. ester extraction and impurity removal; C. extracting with methanol; D. concentrating and washing to obtain a mangiferin crude product with the purity of 60-70 percent: and further carrying out step E and crystallization purification to obtain a mangiferin pure product with the purity of 90-98%. The extraction method can obtain mangiferin with higher purity by adopting a simple extraction and separation means of a plurality of steps, and has the advantages of simple and convenient operation and greatly reduced cost. The extraction method can respectively obtain a mangiferin crude product with the purity of 60-70% and a mangiferin pure product with the purity of 90-98%, wherein the yield of the mangiferin crude product is more than or equal to 83%, and the yield of the pure product is more than or equal to 65%.
Description
Technical Field
The invention belongs to the field of plant extraction, and particularly relates to a method for extracting and separating mangiferin from mango leaves.
Background
Mangiferin is a carbon ketoside of tetrahydroxypyranone, and has a molecular formula of C19H18O11The structural formula is shown as formula 1, and the mangosteen extract is widely applied to various plants such as mangoes, rhizoma anemarrhenae, herba artemisiae scopariae, swertia davidi and the like. In Chinese pharmacopoeia and quality standards of various traditional Chinese medicinal materials and Chinese patent medicines, the content of mangiferin is widely used as a quality control index. Modern medical research proves that mangiferin has the functions of resisting oxidation, inflammation and radiation, preventing and treating skin aging, reducing blood sugar and uric acid,Has pharmacological actions in various aspects such as anti-tumor, immunoregulation and the like, and has extremely high development and utilization prospects.
Mango (Mangifera indica L.) is a common tropical fruit in southern regions of China. The mango planting area in the Panxi region in Sichuan is more than 30 ten thousand mu, the mango planting area has the characteristics of high yield and good quality, the mango planting area occupies the domestic late-maturing mango market, and the mango industry becomes the leading industry of local agriculture. Long-term test analysis shows that the content of mangiferin in mango leaves in the Panxi region is as high as 2-8%, is far higher than that of other plants such as rhizoma anemarrhenae and is also far higher than that of mangiferin in mango leaves in other production regions in China. The mangiferin is efficiently extracted and separated from the local rich mango leaf resources, so that the economic benefit of the local mango industry can be greatly improved, and the method has important significance for reducing the cost of mangiferin raw material medicines and promoting the further development and utilization of the mangiferin.
The existing method for extracting and separating mangiferin from mango leaves is complex in general process, generally obtains a product with the purity of more than 80% by chromatographic separation, and is high in extraction cost. The invention provides a simple method for obtaining mangiferin with high purity.
Disclosure of Invention
The technical problem solved by the invention is to provide a brand-new method for extracting and separating mangiferin from mango leaves, which is simple and easy to operate and can obtain mangiferin with higher purity.
The method for extracting and separating mangiferin from mango leaves comprises the following steps:
A. preparing raw materials: drying mango leaves serving as a raw material, crushing, and sieving with a 20-40-mesh sieve to obtain mango leaf powder;
B. ester extraction and impurity removal: weighing mango leaf powder, adding 2-4L ethyl acetate into each kilogram of mango leaf powder, sealing and soaking for more than or equal to 4h, shaking at room temperature for more than or equal to 10min, and filtering; repeatedly extracting for 3-5 times until the green color of the extractive solution is almost disappeared to obtain mango leaf residue;
C. methanol extraction: taking the mango leaf residue extracted in the step B, adding 2-4L of methanol into each kilogram of mango leaf residue, sealing and soaking for more than or equal to 4 hours at the temperature of 30-40 ℃, stirring and extracting for 0.5-1 hour at the temperature of 50-60 ℃, filtering while hot, repeatedly extracting for 4-6 times, combining extracting solutions, precipitating at room temperature for more than or equal to 8 hours, and filtering to obtain a filtrate;
D. concentration and washing: concentrating the filtrate obtained in the step C into a thick extract, adding 2-4L of methanol into each kilogram of extract, stirring and washing at 50-60 ℃, cooling, filtering, and repeatedly washing for 3-5 times until filter residues are yellow-white particles; drying the filter residue to obtain a mangiferin crude product with the purity of 60-70%.
Further, in order to obtain mangiferin with higher purity, the mangiferin crude product obtained in the step D can be crystallized and purified. E, crystallization purification: taking the mangiferin crude product obtained in the step D, adding 3-5L of 40-60% (Vol) ethanol into each kilogram of mangiferin crude product, stirring and washing for 10min at 50-60 ℃, cooling for more than or equal to 4h at 4-10 ℃, filtering, and repeating for 3-5 times; drying the filter residue to obtain a pure mangiferin product with the purity of 90-98%.
In the technical scheme, fresh mango leaves are adopted as the mango leaves in the step A; in particular, fresh mango tender leaves are adopted as the mango leaves in the step A. However, in view of the collection of the raw materials, young leaves of mango, old leaves at the base of the shoot, and a mixture thereof are generally used. This is because the inventors found: the mango leaf content in mango leaves of different varieties and old tender degrees is greatly different, for example, the content of Kate, Haiton, Jilu and other varieties with large planting areas is generally 2-4%, the content of traditional old varieties such as Miscanthus sinensis and the like can be as high as 6-8%, and the content of tip tender leaves of the same variety is far higher than that of old leaves at the base of branches. Therefore, the raw materials used in the extraction method mainly comprise tender leaves of various mangos, old leaves at the base of branches and mixtures thereof, and fresh mango leaves can be collected as mixed raw materials during flower thinning and fruit thinning or during pruning after mango harvesting.
In the technical scheme, the drying in the step A is natural drying or drying at 45-65 ℃ until the moisture content is less than 8%.
In the technical scheme, the room temperature precipitation in the step C is filtered for more than or equal to 8 hours, and a filter screen with more than or equal to 200 meshes is adopted for fine filtration.
In the technical scheme, the filtrate obtained in the step D is concentrated by vacuum rotary evaporation at the temperature of 5-65 ℃.
In the technical scheme, the step D is stirred and washed for 10-20min at 50-60 ℃.
In the technical scheme, the filtering in the step D adopts a filter screen with the mesh size of more than or equal to 200.
In the technical scheme, the drying in the step D is drying at 50-60 ℃.
In the technical scheme, the step E of crystallization and purification adopts a filter screen with the mesh size of more than or equal to 200 for filtration.
In the technical scheme, the drying filter residue in the step E is dried filter residue at 50-60 ℃.
The key steps and the functions of the invention are as follows: the purpose of the step B is to remove fat-soluble components in mango leaves through ethyl acetate extraction, the fat-soluble components can seriously hinder the precipitation of a mangiferin product in the subsequent step, and the loss rate of the mangiferin in the step is less than 2%. And step C, extracting by utilizing the characteristic that mangiferin is dissolved in hot methanol, wherein the yield is more than or equal to 95%. And D, washing the mangiferin in the concentrated extract by using the principle that the mangiferin is dissolved in hot methanol and has extremely low solubility in cold methanol to obtain a mangiferin crude product with the purity of more than or equal to 60 percent, wherein the yield of the step is more than or equal to 90 percent. And E, crystallizing and purifying by using the principle that mangiferin is dissolved in hot dilute ethanol and has extremely low solubility in cold dilute ethanol to obtain a mangiferin pure product with the purity of more than or equal to 90 percent, wherein the yield of the step is more than or equal to 80 percent.
The extraction method has the beneficial effects that the mangiferin with higher purity can be obtained by adopting a simple extraction and separation means of a plurality of steps, the operation is simple and convenient, and the cost is greatly reduced. The extraction method can respectively obtain a mangiferin crude product with the purity of 60-70% and a mangiferin pure product with the purity of 90-98%, wherein the yield of the mangiferin crude product is more than or equal to 83%, and the yield of the pure product is more than or equal to 65%.
Detailed Description
The present invention will be described in further detail below with reference to specific embodiments of examples, but the present invention is not limited thereto.
The inventor adopts high performance liquid chromatography to precisely determine that: the content of the mangiferin in mango leaves in the Panxi region is as high as 2-8%, which is far higher than that in other plants such as rhizoma anemarrhenae and the like, and is also far higher than that in mango leaves in other production regions in China. The mango leaf content in mango leaves of different varieties and old tender degrees is greatly different, for example, the content of Kate, Haiton, Jilu and other varieties with large planting areas is generally 2-4%, the content of traditional old varieties such as Miscanthus sinensis and the like can be as high as 6-8%, and the content of tip tender leaves of the same variety is far higher than that of old leaves at the base of branches.
The advantageous effects of the present invention are illustrated by the following preparation examples of the present invention.
Example 1
A. Preparing raw materials: fresh mango leaves are taken as raw materials, naturally dried in the sun or dried at 50 ℃, crushed and sieved by a 20-mesh sieve.
B. Ester extraction and impurity removal: weighing 1000g of mango leaf powder, adding 3L of ethyl acetate, sealing and soaking for 5h, shaking and extracting at room temperature for 15min, and filtering; the extraction is repeated for 4 times, and the green color of the extractive solution basically disappears.
C. Methanol extraction: and D, adding 2.5L of methanol into the residue extracted in the step B, soaking for 5h at 30 ℃ in a sealed manner, stirring and extracting for 0.5h at 55 ℃, filtering while hot, repeatedly extracting for 5 times, combining the extracting solutions, precipitating for 9h at room temperature, and finely filtering by using a 200-mesh filter screen.
D. Concentration and washing: and C, carrying out vacuum rotary evaporation and concentration on the filtrate obtained in the step C at 50 ℃ to obtain about 50g of concentrated extract, adding 150mL of methanol, stirring and washing for 10min at 55 ℃, cooling, filtering by using a 200-mesh filter screen, and repeatedly washing for 4 times, wherein filter residues are yellow-white particles. Drying the filter residue at 55 ℃ to obtain a mangiferin crude product with the purity of 62.5 percent, wherein the yield is about 84.5 percent.
Example 2
A. Preparing raw materials: fresh mango leaves are used as raw materials, naturally dried in the sun, crushed and sieved by a 30-mesh sieve.
B. Ester extraction and impurity removal: weighing 1000g of mango leaf powder, adding 4L of ethyl acetate, sealing and soaking for 4h, shaking at room temperature for 10min, and filtering; the extraction is repeated for 3 times, and the green color of the extractive solution basically disappears.
C. Methanol extraction: and D, adding 4L of methanol into the residue extracted in the step B, hermetically soaking at 40 ℃ for 4h, stirring and extracting at 60 ℃ for 0.5h, filtering while hot, repeatedly extracting for 4 times, combining the extracting solutions, precipitating at room temperature for 10h, and finely filtering by using a 200-mesh filter screen.
D. Concentration and washing: and C, carrying out vacuum rotary evaporation on the filtrate obtained in the step C at 65 ℃ to concentrate the filtrate into a thick extract, adding 200mL of methanol, stirring and washing at 50 ℃ for 20min, cooling, filtering by using a 200-mesh filter screen, repeatedly washing for 5 times, and enabling filter residues to be yellow-white particles. Drying the filter residue at 50 ℃ to obtain 43.4g of mangiferin crude product with the purity of 67.6%.
E. And (3) crystallization and purification: and D, adding 160mL of 45% ethanol into the mangiferin crude product obtained in the step D, stirring and washing at 55 ℃ for 10min, cooling in a refrigerator at 4-6 ℃ for 4h, filtering by using a 200-mesh filter screen, and repeating for 3 times. Drying the filter residue at 50 ℃ to obtain 26.5g of a mangiferin pure product with the purity of 92.4%, wherein the yield is 71.2%.
Example 3
A. Preparing raw materials: fresh mango leaves are taken as raw materials, dried at 65 ℃, crushed and sieved by a 40-mesh sieve.
B. Ester extraction and impurity removal: weighing 1000g of mango leaf powder, adding 2L of ethyl acetate, sealing and soaking for 6h, shaking at room temperature for 20min, and filtering; the extraction is repeated for 5 times, and the green color of the extractive solution basically disappears.
C. Methanol extraction: and D, adding 2L of methanol into the residue extracted in the step B, soaking for 6h at 30 ℃ in a sealed manner, stirring and extracting for 1h at 60 ℃, filtering while hot, repeatedly extracting for 6 times, combining the extracting solutions, precipitating for 12h at room temperature, and finely filtering by using a 200-mesh filter screen.
D. Concentration and washing: and C, carrying out vacuum rotary evaporation on the filtrate obtained in the step C at 65 ℃ to concentrate the filtrate into a thick extract, adding 130mL of methanol, stirring and washing at 50 ℃ for 20min, cooling, filtering by using a 200-mesh filter screen, repeatedly washing for 5 times, and enabling filter residues to be yellow-white particles. Drying the filter residue at 60 ℃ to obtain 48.2g of a mangiferin crude product with the purity of 66.5%.
E. And (3) crystallization and purification: and D, taking the mangiferin crude product obtained in the step D, adding 20mL of 40-60% ethanol according to the weight volume ratio, stirring and washing at 60 ℃ for 10min, cooling at 6-10 ℃ for 8h, filtering with a 200-mesh filter screen, and repeating for 5 times. Drying the filter residue at 60 ℃ to obtain 25.9g of the mangiferin pure product with the purity of 97.7 percent, wherein the yield is 65.8 percent.
Claims (12)
1. The method for extracting and separating mangiferin from mango leaves is characterized by comprising the following steps of: the method comprises the following steps:
A. preparing raw materials: drying mango leaves serving as a raw material, crushing, and sieving with a 20-40-mesh sieve to obtain mango leaf powder;
B. ester extraction and impurity removal: weighing mango leaf powder, adding 2-4L ethyl acetate into each kilogram of mango leaf powder, sealing and soaking for more than or equal to 4h, shaking at room temperature for more than or equal to 10min, and filtering; repeatedly extracting for 3-5 times until the green color of the extractive solution is almost disappeared to obtain mango leaf residue;
C. methanol extraction: taking the mango leaf residue extracted in the step B, adding 2-4L of methanol into each kilogram of mango leaf residue, sealing and soaking for more than or equal to 4 hours at the temperature of 30-40 ℃, stirring and extracting for 0.5-1 hour at the temperature of 50-60 ℃, filtering while hot, repeatedly extracting for 4-6 times, combining extracting solutions, precipitating at room temperature for more than or equal to 8 hours, and filtering to obtain a filtrate;
D. concentration and washing: concentrating the filtrate obtained in the step C into a thick extract, adding 2-4L of methanol into each kilogram of extract, stirring and washing at 50-60 ℃, cooling, filtering, and repeatedly washing for 3-5 times until filter residues are yellow-white particles; drying the filter residue to obtain a mangiferin crude product with the purity of 60-70%;
E. and (3) crystallization and purification: taking the mangiferin crude product obtained in the step D, adding 3-5L of 40-60% ethanol in volume concentration per kilogram of the mangiferin crude product, stirring and washing for 10min at 50-60 ℃, cooling for more than or equal to 4h at 4-10 ℃, filtering, and repeating for 3-5 times; drying the filter residue to obtain a pure mangiferin product with the purity of 90-98%.
2. The method for extracting and separating mangiferin from mango leaves as claimed in claim 1, wherein the method comprises the following steps: at least one of the following is satisfied:
adopting fresh mango leaves as the mango leaves in the step A;
and the drying in the step A is natural drying or drying at 45-65 ℃ until the moisture content is less than 8%.
3. The method for extracting and separating mangiferin from mango leaves as claimed in claim 2, wherein the method comprises the following steps: and B, adopting fresh mango tender leaves as the mango leaves in the step A.
4. The method for extracting and separating mangiferin from mango leaves as claimed in claim 2, wherein the method comprises the following steps: the mango leaves in the step A adopt tender leaves of mangoes, old leaves at the bases of branches and mixtures thereof.
5. The method for extracting and separating mangiferin from mango leaves as claimed in claim 2, wherein the method comprises the following steps: and the mango leaves in the step A adopt fresh mango leaves collected in a flower thinning and fruit thinning period or a pruning period after mango collection as raw materials.
6. The method for extracting and separating mangiferin from mango leaves as claimed in claim 1, wherein the method comprises the following steps: and C, filtering the room temperature precipitate for more than or equal to 8 hours, and finely filtering by using a filter screen with more than or equal to 200 meshes.
7. The method for extracting and separating mangiferin from mango leaves as claimed in claim 1, wherein the method comprises the following steps: and D, concentrating the filtrate by adopting vacuum rotary evaporation at 5-65 ℃.
8. The method for extracting and separating mangiferin from mango leaves as claimed in claim 1, wherein the method comprises the following steps: and D, stirring and washing for 10-20min at 50-60 ℃.
9. The method for extracting and separating mangiferin from mango leaves as claimed in claim 1, wherein the method comprises the following steps: and D, filtering by using a filter screen with the mesh size of more than or equal to 200.
10. The method for extracting and separating mangiferin from mango leaves as claimed in claim 1, wherein the method comprises the following steps: and D, drying at 50-60 ℃.
11. The method for extracting and separating mangiferin from mango leaves as claimed in claim 1, wherein the method comprises the following steps: and E, crystallizing and purifying, wherein the filtering is performed by using a filter screen with the mesh size of more than or equal to 200.
12. The method for extracting and separating mangiferin from mango leaves as claimed in claim 1, wherein the method comprises the following steps: and E, drying the filter residue at 50-60 ℃.
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| CN111423424B (en) * | 2020-01-20 | 2021-12-14 | 中国热带农业科学院分析测试中心 | Preparation method of high-purity mangiferin crystal |
| CN113416182B (en) * | 2021-05-28 | 2022-03-29 | 西安金泰生物技术有限公司 | Mangiferin and preparation method thereof |
| CN113429401A (en) * | 2021-07-06 | 2021-09-24 | 蒙汉富 | Mangiferin extraction and separation method |
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| CN101671330A (en) * | 2009-10-13 | 2010-03-17 | 刘全胜 | Preparation method of mangiferin |
| CN102408415A (en) * | 2010-09-21 | 2012-04-11 | 昆明制药集团股份有限公司 | Preparation method of mangiferin |
| CN103768112A (en) * | 2012-10-26 | 2014-05-07 | 昆明制药集团股份有限公司 | Mango leaf extract and application thereof |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101671330A (en) * | 2009-10-13 | 2010-03-17 | 刘全胜 | Preparation method of mangiferin |
| CN102408415A (en) * | 2010-09-21 | 2012-04-11 | 昆明制药集团股份有限公司 | Preparation method of mangiferin |
| CN103768112A (en) * | 2012-10-26 | 2014-05-07 | 昆明制药集团股份有限公司 | Mango leaf extract and application thereof |
Non-Patent Citations (1)
| Title |
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| 四川攀西干热河谷区芒果叶中芒果苷含量变化规律研究;韦会平，等;《南方农业学报》;20161231;第47卷(第12期);第2134-2138页 * |
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