CN1157353C - Method of refining effective component of official magnolia - Google Patents
Method of refining effective component of official magnolia Download PDFInfo
- Publication number
- CN1157353C CN1157353C CNB011301295A CN01130129A CN1157353C CN 1157353 C CN1157353 C CN 1157353C CN B011301295 A CNB011301295 A CN B011301295A CN 01130129 A CN01130129 A CN 01130129A CN 1157353 C CN1157353 C CN 1157353C
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- China
- Prior art keywords
- magnolol
- honokiol
- temperature
- vacuum tightness
- boiling point
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Abstract
The present invention relates to magnolol as an effective ingredient of magnolia bark and a refining method of honokiol. The refining method is characterized in that magnolia bark extract with a total content 10.0 to 50.0% of magnolol and honokiol as raw material is treated through molecular distillation at a vacuum degree of 20 to 50Pa and temperature of 80 to 120 DEG C, and then at a vacuum degree of 1 to 5Pa and temperature of 100 to 250 DEG C to obtain a semi-crystalline or crystalline product. With the method of the present invention, magnolol and honokiol have the recovery rate over 90%, the content of 80.0 to 99.0% and no residue solvent, etc., and can be directly used as raw material intermediates used in the fields of oral cavity health-care products, traditional Chinese medicines and pharmacies, etc.
Description
Technical field
The present invention relates to a kind of process for purification of effective ingredient.
Background technology
The dry hide of the Magnoliacea plant bark of official magnolia (Magnolia officinalis Rehd.et Wils.) or Magnolia bilola (M.officinalis Rehd.et Wils.var.biloba Rehd.et Wils.), Gen Pi and the contained bark of official magnolia effective constituent of branch skin have warm in nature, flavor is hot, bitter, the energy warming middle-JIAO to promote flow of QI, eliminating dampness is removed full, be used for the treatment of taste and hinder in cold-dampness, wrist distention and fullness in the abdomen or pain symptoms such as anorexia, four limbs burnout.Modern pharmacological research shows that magnolia bark preparation has restraining effect to streptococcus pneumoniae, alpha streptococcus, beta streptococcus, dysentery bacterium, Corynebacterium diphtheriae, intestinal bacteria, streptococcus aureus, cholera fox bacterium, paratyphosum Bacterium etc.Magnolol and Honokiol also have the maincenter myorelaxant effects.
Contain about 5～15% magnolols (magnolol) and Honokiol (honokiol) in the Magnoliacea plant bark of official magnolia, about 1% Cortex Magnoliae Officinalis volatile oil, contain the low boiling point component about 95% in the oil, as β-eucalyptol (β-eudesmol) and a spot of α-Pai Xi (α-pinene), and tetrahydromagnolol (tetrahydromagnolol), iso-agnolol (isomagnolol) etc., also contain about about 0.07% high boiling point composition, as l-magnocurarine alkaloids such as (magnocurarine), about 0.45% saponin, tannin and micro-nicotinic acid etc.
The traditional method of bark of official magnolia refining effective ingredients mainly is a solvent crystallization, but the solvent crystallization method exists that the rate of recovery is low, cost is high and problem such as dissolvent residual.
Summary of the invention
Having the objective of the invention is to propose one is that 10.0～50.0% Cortex Magnoliae Officinalis extract is a raw material with magnolol and Honokiol total content, adopts molecular distillation technique, directly obtains hypocrystalline or crystalline method.
The present invention implements as follows: the Cortex Magnoliae Officinalis extract with magnolol and Honokiol total content 10.0～50.0% is a raw material, and at vacuum tightness 20～50Pa, 80～120 ℃ of following molecular distillations of temperature are removed low boiling point component; At vacuum tightness 1～5Pa, 100～250 ℃ of following molecular distillations of temperature are removed the high boiling point composition, obtain hypocrystalline or crystallized product then.
Preferred molecular distillation condition is respectively vacuum tightness 25～40Pa, 100～120 ℃ of temperature; Vacuum tightness 2～4Pa, 150～210 ℃ of temperature.
Best molecular distillation condition is vacuum tightness 3Pa, 120 ℃ of temperature; Vacuum tightness 3Pa, 180 ℃ of temperature.
Method of the present invention compared with prior art, the rate of recovery is more than 90%, magnolol and Honokiol content is 80.0～99.0%, problems such as no solvent residue.The product that this method obtains can directly be used for fields such as oral care product, Chinese materia medica as raw material midbody.
Embodiment
The invention will be further described below in conjunction with embodiment.
Embodiment 1
Get Cortex Magnoliae Officinalis extract 100.0g, magnolol and Honokiol content 10%, under pressure, temperature are respectively 30Pa, 100 ℃, carry out molecular distillation and remove low boiling point component, debris 20.0g carries out molecular distillation again and removes the high boiling point composition under 1Pa, 100 ℃, can obtain product 10.5g, magnolol and Honokiol content 90.0%, the rate of recovery 94.5%.
Embodiment 2
Get Cortex Magnoliae Officinalis extract 100.0g, magnolol and Honokiol content 20%, under pressure, temperature are respectively 20Pa, 80 ℃, carry out molecular distillation and remove low boiling point component, debris 28.2g carries out molecular distillation again and removes the high boiling point composition under 5Pa, 150 ℃, can obtain product 23.0g, magnolol and Honokiol content 85.0%, the rate of recovery 97.8%.
Embodiment 3
Get Cortex Magnoliae Officinalis extract 100.0g, magnolol and Honokiol content 30%, under pressure, temperature are respectively 30Pa, 85 ℃, carry out molecular distillation and remove low boiling point component, debris 42.5g carries out molecular distillation again and removes the high boiling point composition under 2Pa, 180 ℃, can obtain product 36.9g, magnolol and Honokiol content 80.0%, the rate of recovery 98.4%.
Embodiment 4
Get Cortex Magnoliae Officinalis extract 100g, magnolol and Honokiol content 40%, under pressure, temperature are respectively 25Pa, 90 ℃, carry out molecular distillation and remove low boiling point component, debris 45.2g carries out molecular distillation again and removes the high boiling point composition under 3Pa, 250 ℃, can obtain product 41.0g, magnolol and Honokiol content 88.0%, the rate of recovery 90.2%.
Embodiment 5
Get Cortex Magnoliae Officinalis extract 100g, magnolol and Honokiol content 50%, under pressure, temperature are respectively 35Pa, 110 ℃, carry out molecular distillation and remove low boiling point component, debris 56.2g carries out molecular distillation again and removes the high boiling point composition under 3Pa, 220 ℃, can obtain product 50.5g, magnolol and Honokiol content 93.0%, the rate of recovery 93.9%.
Embodiment 6
Get Cortex Magnoliae Officinalis extract 100.0g, magnolol and Honokiol content 50%, under pressure, temperature are respectively 40Pa, 115 ℃, carry out molecular distillation and remove low boiling point component, debris 56.0g carries out molecular distillation again and removes the high boiling point composition under 2Pa, 150 ℃, can obtain product 45.4g, magnolol and Honokiol content 99.0%, the rate of recovery 90.1%.
Embodiment 7
Get Cortex Magnoliae Officinalis extract 100.0g, magnolol and Honokiol content 50%, under pressure, temperature are respectively 50Pa, 120 ℃, carry out molecular distillation and remove low boiling point component, debris 55.0g carries out molecular distillation again and removes the high boiling point composition under 3Pa, 190 ℃, can obtain product 48.5g, magnolol and Honokiol content 95.0%, the rate of recovery 92.2%.
Embodiment 8
Get Cortex Magnoliae Officinalis extract 10.0kg, magnolol and Honokiol content 50%, under pressure, temperature are respectively 30Pa, 120 ℃, carry out molecular distillation and remove low boiling point component, debris 5.3kg carries out molecular distillation again and removes the high boiling point composition under 3Pa, 180 ℃, can obtain product 4.72kg, magnolol and Honokiol content 96.5%, the rate of recovery 91.1%.
Claims (3)
1. the method for refining bark of official magnolia effective constituent magnolol and Honokiol, it is characterized in that the Cortex Magnoliae Officinalis extract with magnolol and Honokiol total content 10.0～50.0% is a raw material, at vacuum tightness 20～50Pa, 80～120 ℃ of following molecular distillations of temperature are removed low boiling point component; At vacuum tightness 1～5Pa, 100～250 ℃ of following molecular distillations of temperature are removed the high boiling point composition, obtain magnolol and Honokiol hypocrystalline or crystallized product then.
2. the method for refining bark of official magnolia effective constituent magnolol according to claim 1 and Honokiol is characterized in that preferred molecular distillation condition is respectively vacuum tightness 25～40Pa, 100～120 ℃ of temperature; Vacuum tightness 2～4Pa, 150～210 ℃ of temperature.
3. the method for refining bark of official magnolia effective constituent magnolol according to claim 1 and Honokiol is characterized in that best molecular distillation condition is vacuum tightness 3Pa, 120 ℃ of temperature; Vacuum tightness 3Pa, 180 ℃ of temperature.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB011301295A CN1157353C (en) | 2001-12-27 | 2001-12-27 | Method of refining effective component of official magnolia |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB011301295A CN1157353C (en) | 2001-12-27 | 2001-12-27 | Method of refining effective component of official magnolia |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1362395A CN1362395A (en) | 2002-08-07 |
| CN1157353C true CN1157353C (en) | 2004-07-14 |
Family
ID=4669756
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNB011301295A Expired - Fee Related CN1157353C (en) | 2001-12-27 | 2001-12-27 | Method of refining effective component of official magnolia |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1157353C (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP1837392A1 (en) * | 2006-03-21 | 2007-09-26 | Chanel Parfums Beauté | Oil of magnolia champaca, method for its preparation and compositions containing same |
| WO2007107856A1 (en) * | 2006-03-21 | 2007-09-27 | Chanel Parfums Beaute | Magnolia champaca oil, its process of preparation and compositions comprising it |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115260006B (en) * | 2022-08-07 | 2023-12-12 | 南宁厚新生物科技有限公司 | Method for separating and purifying magnolol and honokiol in magnolia bark extract by molecular distillation |
-
2001
- 2001-12-27 CN CNB011301295A patent/CN1157353C/en not_active Expired - Fee Related
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP1837392A1 (en) * | 2006-03-21 | 2007-09-26 | Chanel Parfums Beauté | Oil of magnolia champaca, method for its preparation and compositions containing same |
| WO2007107856A1 (en) * | 2006-03-21 | 2007-09-27 | Chanel Parfums Beaute | Magnolia champaca oil, its process of preparation and compositions comprising it |
Also Published As
| Publication number | Publication date |
|---|---|
| CN1362395A (en) | 2002-08-07 |
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| Date | Code | Title | Description |
|---|---|---|---|
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C06 | Publication | ||
| PB01 | Publication | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| C17 | Cessation of patent right | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20040714 Termination date: 20100127 |