CN102746121B - Refining method of high purity borneol - Google Patents
Refining method of high purity borneol Download PDFInfo
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- CN102746121B CN102746121B CN201110099748.8A CN201110099748A CN102746121B CN 102746121 B CN102746121 B CN 102746121B CN 201110099748 A CN201110099748 A CN 201110099748A CN 102746121 B CN102746121 B CN 102746121B
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Abstract
The invention relates to a refining method of high purity borneol. The method comprises the following steps: 1, dissolving crude borneol in a solvent acetone; 2, filtering, and cooling the resulting filtrate to crystallize; 3, filtering the resulting crystalline liquid, and drying to obtain first purified borneol; 4, dissolving the first purified borneol in the solvent acetone; 5, filtering, and cooling the resulting filtrate to crystallize; and 6, filtering the resulting crystalline liquid, and drying to obtain pure borneol.
Description
Technical field
The present invention relates to a kind of medical art, be specifically related to a kind of purification process for the treatment of have one's ideas straightened out inducing resuscitation, the Chinese medicine borneol (borneolum syntheticum) of clearing away heat to and alleviating pain.
Background technology
Borneol, has another name called borneol, Borneolum, borneol, and ancient title Dipterocarpus pilosus, being the processing crystallization product of Dipterocarpaceae aiphyllium Borneolum Syntheticum resin, is one of conventional Chinese medicine.Natural Broneolum Syntheticum have Dipterocarpus pilosus and Chinese mugwort brain point, the latter be feverfew Herba Blumeae Balsamiferae leaf extract crystallization, Dipterocarpus pilosus is the certified products in borneol, and main component is borneol.Also containing a large amount of isocamphols except borneol, isocamphol is the epimer of borneol.Natural Broneolum Syntheticum is mainly containing borneol, and synthetic borneol is mainly containing borneol and isocamphol.Large with sheet, matter is thin, and look pure white, and matter is crisp, and gas delicate fragrance person is good. with the title BORNEOLUM SYNTHETICUM of the raw material such as turps, camphor through chemosynthesis.Borneol taste is pungent, bitter, cold nature.There is the function of inducing resuscitation of having one's ideas straightened out, clearing heat for detumescence, pain relieving.For losing consciousness, febrile disease unconsciousness due to high fever, apoplexy coma due to blocking of the respiratory system, lose consciousness, middle evil, sore swell and ache, aphtha, swelling and pain in the throat, conjunctival congestion with pain and swelling of the eye, eye illness, swelling and aching of gum etc.Modern for coronary heart diseases and angina pectoris, be one of main component of Compositae Salviae Miltiorrhizae medicine.
Document mentions that the purifying process of borneol mainly contains subliming method, ethanol-water mixed solvent method for refining and dry column chromatography, and literature procedures all has certain shortcoming, and such as production operability is not strong, and product yield is low, and cost is high.
Summary of the invention
The object of this invention is to provide a kind of new borneol process for purification, the method makes raw material with synthetic borneol crude product, through a series of polishing purification step, and obtained high-purity borneol product.
Borneol process for refining of the present invention, comprises the following steps:
(1) take acetone as solvent, crude product borneol is dissolved;
(2) filter, filtrate crystallisation by cooling;
(3) crystal solution is filtered, dry product of must purifying for the first time;
(4) take acetone as solvent, will dissolve by purification borneol for the first time;
(5) filter, filtrate crystallisation by cooling;
(6) crystal solution is filtered, dry sterling borneol.
Wherein
Step (1) needs to carry out heating for dissolving; Also gac can be added according to crude product quality condition; Mass ratio 0.4-1.5: 1 of acetone and crude product borneol;
Filtered while hot is filtered in step (2); Filtrate cooling and stirring Tc is 0-30 DEG C, and the time is 2-12 hour;
In step (3), filter cake is dry under the condition of 20-70 DEG C;
Concrete steps can be:
(1) adopt acetone to be solvent, add crude product borneol and carry out heating for dissolving, be heated to complete molten backflow;
(2) according to crude product quality condition, add a little gac (1%-5%) insulation and decolour half an hour;
(3) filtered while hot; Filtrate cooling and stirring Tc is 0-30 DEG C, time 2-12 hour;
(4) filter, first purification product are dry under the condition of 20-70 DEG C;
(5) first purification product join in acetone and dissolve, and are heated to complete molten backflow;
(6) filtered while hot; Filtrate cooling and stirring Tc is 0-30 DEG C, time 2-12 hour;
(7) filter, fine work is dry under the condition of 20-70 DEG C;
Preferably:
(1) adopt acetone to be solvent, add crude product borneol and carry out heating for dissolving, be heated to complete molten backflow, the mass ratio 0.5: 1 of acetone and crude product borneol;
(2) according to crude product quality condition, add the insulation of 1%-5% gac and decolour half an hour;
(3) filtered while hot; Filtrate cooling and stirring Tc is 0-30 DEG C, time 2-12 hour;
(4) filter, first purification product are dry under the condition of 20-70 DEG C;
(5) first purification product join in acetone and dissolve, and are heated to complete molten backflow;
(6) filtered while hot; Filtrate cooling and stirring Tc is 0-10 DEG C, time 2-6 hour,
(7) filter, fine work is dry under the condition of 30-60 DEG C.
It is even more preferred that
(1) adopt acetone to be solvent, add crude product borneol and carry out heating for dissolving, be heated to complete molten backflow; The mass ratio 0.5: 1 of acetone and crude product borneol;
(2) according to crude product quality condition, add 1% gac insulation and decolour half an hour;
(3) filtered while hot; Filtrate cooling and stirring Tc is 20 DEG C, 8 hours time;
(4) filter, first purification product are dry under the condition of 20 DEG C;
(5) first purification product join in acetone and dissolve, and are heated to complete molten backflow;
(6) filtered while hot; Filtrate cooling and stirring Tc is 20 DEG C, 8 hours time;
(7) filter, fine work is dry under the condition of 20 DEG C.
The invention has the advantages that:
1. easy and simple to handle feasible, mild condition, refining solvent is low toxicity and recyclablely applies mechanically;
2. product appearance color becomes white from canescence;
3. product content is increased to more than 99.5% by 80.0%;
4, product yield is high, and cost is low;
Borneol process for purification of the present invention, low poison solvent is selected to refine borneol crude product the crude product borneol purchasing available content about 80%, simple to operate, be easy to industrialization, after refining, product appearance, content are all greatly improved, more effective than existing process for purification.
Solvent selection of the present invention is through screening acquisition, and screening process is as follows:
Embodiment
By the following examples, further illustrate the present invention, but not as limitation of the present invention.
Embodiment 1
Add 5kg acetone in a kettle., under stirring, add borneol crude product 10kg.Be heated with stirring to entirely molten, add gac 0.1kg, reflux decolour 30 minutes.Filtered while hot, filtrate cooling and stirring crystallization, is chilled to 5 degree, stirs filtration in 4 hours, dry under the condition of 70 DEG C, obtains purification product 7kg for the first time; Add 7kg acetone in a kettle., under stirring, add first purification product.Be heated with stirring to entirely molten, filtered while hot, filtrate cooling crystallization, be chilled to 0 degree, stir filtration in 4 hours, wet product under the condition of 70 DEG C dry 3 hours, obtains borneol finished product 4kg, yield 40.0%.Product colour is white, and detect through HPLC, content is 99.7%.
Embodiment 2
Add 7kg acetone in a kettle., under stirring, add borneol crude product 12kg.Be heated with stirring to entirely molten, add gac 0.2kg, reflux decolour 30 minutes.Filtered while hot, filtrate cooling and stirring crystallization, is chilled to 0 degree, stirs filtration in 2 hours, dry under the condition of 70 DEG C, obtains purification product 8kg for the first time; Add 9kg acetone in a kettle., under stirring, add first purification product.Be heated with stirring to entirely molten, filtered while hot, filtrate cooling crystallization, be chilled to 10 degree, stir filtration in 5 hours, wet product under the condition of 40 DEG C dry 6 hours, obtains borneol finished product 5.5kg, yield 45.8%.Product colour is white, and detect through HPLC, content is 99.6%.
Embodiment 3
Add 5kg acetone in a kettle., under stirring, add borneol crude product 10kg.Be heated with stirring to entirely molten, filtered while hot, filtrate cooling and stirring crystallization, is chilled to 8 degree, stirs filtration in 4 hours, dry under the condition of 20 DEG C, obtains purification product 7.4kg for the first time; Add 7kg acetone in a kettle., under stirring, add first purification product.Be heated with stirring to entirely molten, filtered while hot, filtrate cooling crystallization, be chilled to 5 degree, stir filtration in 4 hours, wet product under the condition of 35 DEG C dry 6 hours, obtains borneol finished product 4.5kg, yield 45.0%.Product colour is white, and detect through HPLC, content is 99.5%.
Embodiment 4
Add 5kg acetone in a kettle., under stirring, add borneol crude product 10kg.Be heated with stirring to entirely molten, add gac 0.1kg, reflux decolour 30 minutes.Filtered while hot, filtrate cooling and stirring crystallization, is chilled to 30 degree, stirs filtration in 12 hours, dry under the condition of 40 DEG C, obtains purification product 6.5kg for the first time; Add 7kg acetone in a kettle., under stirring, add first purification product.Be heated with stirring to entirely molten, filtered while hot, filtrate cooling crystallization, be chilled to 30 degree, stir filtration in 12 hours, wet product under the condition of 20 DEG C dry 10 hours, obtains borneol finished product 4.3kg, yield 43.0%.Product colour is white, and detect through HPLC, content is 99.7%.
Embodiment 5
Add 4kg acetone in a kettle., under stirring, add borneol crude product 10kg.Be heated with stirring to entirely molten, add gac 0.1kg, reflux decolour 30 minutes.Filtered while hot, filtrate cooling and stirring crystallization, is chilled to 30 degree, stirs filtration in 12 hours, dry under the condition of 40 DEG C, obtains purification product 6.5kg for the first time; Add 7kg acetone in a kettle., under stirring, add first purification product.Be heated with stirring to entirely molten, filtered while hot, filtrate cooling crystallization, be chilled to 30 degree, stir filtration in 12 hours, wet product under the condition of 20 DEG C dry 10 hours, obtains borneol finished product 4.6kg, yield 46.0%.Product colour is white, and detect through HPLC, content is 99.6%.
Embodiment 6
Add 15kg acetone in a kettle., under stirring, add borneol crude product 10kg.Be heated with stirring to entirely molten, add gac 0.1kg, reflux decolour 30 minutes.Filtered while hot, filtrate cooling and stirring crystallization, is chilled to 30 degree, stirs filtration in 12 hours, dry under the condition of 40 DEG C, obtains purification product 6.7kg for the first time; Add 7kg acetone in a kettle., under stirring, add first purification product.Be heated with stirring to entirely molten, filtered while hot, filtrate cooling crystallization, be chilled to 30 degree, stir filtration in 12 hours, wet product under the condition of 30 DEG C dry 10 hours, obtains borneol finished product 4.4kg, yield 44.0%.Product colour is white, and detect through HPLC, content is 99.7%.
Embodiment 7
Add 5kg acetone in a kettle., under stirring, add borneol crude product 10kg.Be heated with stirring to entirely molten, add gac 0.5kg, reflux decolour 30 minutes.Filtered while hot, filtrate cooling and stirring crystallization, is chilled to 0 degree, stirs filtration in 2 hours, dry under the condition of 20 DEG C, obtains purification product 6.3kg for the first time; Add 7kg acetone in a kettle., under stirring, add first purification product.Be heated with stirring to entirely molten, filtered while hot, filtrate cooling crystallization, be chilled to 0 degree, stir filtration in 2 hours, wet product under the condition of 20 DEG C dry 10 hours, obtains borneol finished product 4.25kg, yield 42.5%.Product colour is white, and detect through HPLC, content is 99.6%.
Embodiment 8
Add 5kg acetone in a kettle., under stirring, add borneol crude product 10kg.Be heated with stirring to entirely molten, add gac 0.1kg, reflux decolour 30 minutes.Filtered while hot, filtrate cooling and stirring crystallization, is chilled to 10 degree, stirs filtration in 8 hours, dry under the condition of 70 DEG C, obtains purification product 6.4kg for the first time; Add 7kg acetone in a kettle., under stirring, add first purification product.Be heated with stirring to entirely molten, filtered while hot, filtrate cooling crystallization, be chilled to 10 degree, stir filtration in 6 hours, wet product under the condition of 60 DEG C dry 10 hours, obtains borneol finished product 4.35kg, yield 43.5%.Product colour is white, and detect through HPLC, content is 99.5%.
Claims (2)
1. a process for purification for borneol, is characterized in that, comprises the following steps:
(1) adopt acetone to be solvent, add crude product borneol and carry out heating for dissolving, be heated to complete molten backflow; The mass ratio 0.4-1.5:1 of acetone and crude product borneol;
(2) according to crude product quality condition, add the insulation of 1%-5% gac and decolour half an hour;
(3) filtered while hot; Filtrate cooling and stirring Tc is 0-30 DEG C, time 2-12 hour;
(4) filter, first purification product are dry under the condition of 20-70 DEG C;
(5) first purification product join in acetone and dissolve, and are heated to complete molten backflow;
(6) filtered while hot; Filtrate cooling and stirring Tc is 0-30 DEG C, time 2-12 hour;
(7) filter, fine work is dry under the condition of 20-70 DEG C.
2. process for purification according to claim 1, is characterized in that, comprises the following steps:
(1) adopt acetone to be solvent, add crude product borneol and carry out heating for dissolving, be heated to complete molten backflow, the mass ratio 0.5:1 of acetone and crude product borneol;
(2) according to crude product quality condition, add the insulation of 1%-5% gac and decolour half an hour;
(3) filtered while hot; Filtrate cooling and stirring Tc is 0-30 DEG C, time 2-12 hour;
(4) filter, first purification product are dry under the condition of 20-70 DEG C;
(5) first purification product join in acetone and dissolve, and are heated to complete molten backflow;
(6) filtered while hot; Filtrate cooling and stirring Tc is 0-10 DEG C, time 2-6 hour,
(7) filter, fine work is dry under the condition of 30-60 DEG C.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201110099748.8A CN102746121B (en) | 2011-04-20 | 2011-04-20 | Refining method of high purity borneol |
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| CN201110099748.8A CN102746121B (en) | 2011-04-20 | 2011-04-20 | Refining method of high purity borneol |
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| CN102746121A CN102746121A (en) | 2012-10-24 |
| CN102746121B true CN102746121B (en) | 2015-03-25 |
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Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105037098B (en) * | 2015-06-01 | 2016-05-18 | 福建青松股份有限公司 | A kind of new technology of borneolum syntheticum crystalline sheet borneol |
| CN109134192A (en) * | 2017-06-27 | 2019-01-04 | 贵州艾源生态药业开发有限公司 | A kind of extracting method of borneol |
| CN112409134A (en) * | 2020-10-31 | 2021-02-26 | 熊华民 | Extraction and refining process of natural borneol |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN85102398A (en) * | 1985-04-01 | 1986-10-01 | 中国科学院广州化学研究所 | Catalyst for synthesizing pure L-borneol and preparation method and application technology |
| CN1049842A (en) * | 1990-06-05 | 1991-03-13 | 中国科学院广州化学所 | Synthetic method of isoborneol by catalyzing camphenic water with resin |
| CN101386566A (en) * | 2007-09-10 | 2009-03-18 | 吉安市林业科学研究所 | Preparation method of flake crystalline solid natural borneol |
-
2011
- 2011-04-20 CN CN201110099748.8A patent/CN102746121B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN85102398A (en) * | 1985-04-01 | 1986-10-01 | 中国科学院广州化学研究所 | Catalyst for synthesizing pure L-borneol and preparation method and application technology |
| CN1049842A (en) * | 1990-06-05 | 1991-03-13 | 中国科学院广州化学所 | Synthetic method of isoborneol by catalyzing camphenic water with resin |
| CN101386566A (en) * | 2007-09-10 | 2009-03-18 | 吉安市林业科学研究所 | Preparation method of flake crystalline solid natural borneol |
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