CN102557881B - A kind of extraction separation and purification method of L-Borneol - Google Patents
A kind of extraction separation and purification method of L-Borneol Download PDFInfo
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- CN102557881B CN102557881B CN201010579560.9A CN201010579560A CN102557881B CN 102557881 B CN102557881 B CN 102557881B CN 201010579560 A CN201010579560 A CN 201010579560A CN 102557881 B CN102557881 B CN 102557881B
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Abstract
The present invention relates to a kind of extraction and separation method of L-Borneol, specifically belong to technical field of plant extraction deep-processing.Feature gets Herba Blumeae Balsamiferae leaf and spray is that raw material is pulverized, and obtains L-Borneol through Simultaneous distillation extraction, reduction vaporization, Decompression Sublimation separation and purification.The L-Borneol that the present invention extracts reaches the specification of quality of " Chinese Pharmacopoeia 2010 ", and in whole process, L-Borneol extraction rate reached is to 90%, and the rate of recovery reaches 80%; Process for extracting, separating and purifying is easy, and efficiency is high, loses little, and treatment capacity is large, is applicable to suitability for industrialized production; And can technical support be provided for the extraction separation and purification of L-Borneol and provide natural high quality raw material for medicine, medical and beauty treatment and essence and flavoring agent industry.
Description
Technical field
The present invention relates to a kind of L-Borneol extraction separation and purification method, specifically belong to technical field of plant extraction deep-processing.
Background technology
L-Borneol, also known as Chinese mugwort brain, L-Borneol or L-Borneol etc., be the one of borneol, borneol is divided three classes by " Chinese Pharmacopoeia 2010 ", i.e. L-Borneol, natural Broneolum Syntheticum and synthetic borneol.L-Borneol extracts to obtain from the leaf and spray of composite family Herba Blumeae Balsamiferae platymiscium Herba Blumeae Balsamiferae (Blumeabalsamifera (L.) DC.), there is inducing resuscitation of having one's ideas straightened out, clearing away heat to and alleviating pain effect, faint for pyreticosis coma, convulsion, apoplexy coma due to blocking of the respiratory system, the obstruction of the circulation of vital energy is fainted cruelly, middle evil stupor, hot eyes, aphtha, swelling and pain in the throat, duct is suppurated, and is the important component part of multiple Chinese patent medicine and ethnic drug (seedling medicine).L-Borneol main component is L-Borneol, and L-Borneol (L-borneol) chemical name is L-2-baras camphor or L-inner mold-1,7,7-trimethylammonium two ring [2.2.1]-2-in heptan alcohol, and molecular formula is C
10h
17oH, structural formula is:
Modern study finds that L-Borneol has bacteriostatic action, and effect is better than d-Bomeol; Also have and promote Drug Percutaneous Absorption, effect through hemato encephalic barrier and blood-eye barrier, Plasma Concentration and the bioavailability of other drug can be improved.L-Borneol has widespread use in industries such as medicine, medical and beauty treatment and essence and flavoring agents and is worth.
Existing L-Borneol technique of producing is traditional steam distillation, and through the development of decades, technical process is substantially unchanged, and just processing units improves to some extent.Do not find that Herba Blumeae Balsamiferae extracts the relevant report of L-Borneol abroad in document, at home in bibliographical information, river Xing Long in 2006 etc. introduce the place of production and gather and extract Chinese mugwort powder technology, and this technology is processing L-Borneol precursor substance Chinese mugwort powder just.In patent, Tropical Crop Variety Resource Institute of Chinese Academy of Tropical Agricultural Sciences obtains " Chinese mugwort powder extraction element ", " a kind of Herba Blumeae Balsamiferae processing extraction equipment " two utility model patent mandates respectively 2009 and 2010, these two kinds of devices are all manufacture and design on extraction by steam distillation L-Borneol Process ba-sis, do not propose novel process.Traditional method does not process Herba Blumeae Balsamiferae raw material, and large at distillation hourly water consumption, extraction efficiency is low; In the course of processing, loss of material is serious, distillation and sublimation apparatus operating temperature high, L-Borneol transform and degraded seriously; Equipment falls behind, and labour intensity is large.For overcoming the shortcoming that traditional method exists, the present invention pulverizes raw material, is conducive to improving extraction efficiency; Adopt Simultaneous distillation during extraction, water consumption is few, and extraction fully; Reduction vaporization and Decompression Sublimation process temperature low, reduce L-Borneol degraded and transform risk, improve the rate of recovery.
Summary of the invention
The object of the invention is to the deficiency overcoming traditional method, a kind of extraction separation and purification method of L-Borneol is provided, utilize Herba Blumeae Balsamiferae leaf and spray to be raw material, obtain the L-Borneol meeting " Chinese Pharmacopoeia 2010 " and require; Process for extracting, separating and purifying is simple, and extract fully, extraction efficiency is high, and loss of material is little, and treatment capacity is large, is applicable to suitability for industrialized production.
According to technical scheme provided by the invention, a kind of extraction separation and purification method of L-Borneol, adopts following processing step:
(1) raw material: getting Herba Blumeae Balsamiferae is that raw material is pulverized, and grinding particle size is 0.1 ~ 1mm;
(2) Simultaneous distillation-extraction: the Herba Blumeae Balsamiferae powder-material after pulverizing is added to the water, be heated to micro-generation water vapor that boils, micro-the boiling of heat oil ether produces sherwood oil steam simultaneously, the fat-soluble volatile component that when two-phase steam meets, sherwood oil steam extraction water vapor carries, both are condensation simultaneously in prolong, because water and the immiscible property of sherwood oil make both be separated, wherein distilling aqueous phase is back in water bottle, sherwood oil is back in sherwood oil bottle mutually, obtain Herba Blumeae Balsamiferae petroleum ether extract, whole process is 5 ~ 10h;
(3) reduction vaporization: Herba Blumeae Balsamiferae petroleum ether extract is evaporated under reduced pressure atmosphere, pressure is 0.01 ~ 0.09MPa, temperature is 10 ~ 30 DEG C, time is 0.5 ~ 2h, obtain Herba Blumeae Balsamiferae volatile component, the sherwood oil that evaporation is reclaimed can reuse, and saves material, and cold operation reduces the loss of L-Borneol in volatile component and transforms risk;
(4) Decompression Sublimation: L-Borneol crude product is carried out Decompression Sublimation, pressure is 0.01 ~ 0.09MPa, and temperature is 50 ~ 150 DEG C, and the time is 1 ~ 10h, collect crystal in condenser and namely obtain L-Borneol, the operating temperature lower than atmospheric sublimation reduces the risk that L-Borneol transforms and degrades.
Described L-Borneol is composite family Herba Blumeae Balsamiferae platymiscium Herba Blumeae Balsamiferae (Latin is called Blumeabalsamifera (L.) DC.), originates in Luodian County, Guizhou Province.
Described L-Borneol is included in " Chinese Pharmacopoeia 2010 ", L-Borneol content >=85% in L-Borneol, isocamphol content≤5%, camphor content≤10%.
Compared with the prior art the present invention has the following advantages:
The present invention uses Simultaneous distillation in leaching process, due to water and sherwood oil immiscible, can layering backflow, this method comparatively traditional method reduces water consumption in a large number, and sherwood oil consumption is also quite few, and the application of sherwood oil makes extraction abundant, improves extraction efficiency; When reduction vaporization, use the operating temperature lower than normal pressure to reclaim sherwood oil, both ensured that L-Borneol was stablized, ensure again recycling sherwood oil; When Decompression Sublimation, use the temperature lower than atmospheric sublimation to be separated L-Borneol from crude product, reduce L-Borneol Yin Gaowen and distil the conversion or degraded that cause, the raising L-Borneol rate of recovery; The L-Borneol that Decompression Sublimation obtains, requirement that quality meets " Chinese Pharmacopoeia 2010 ", in whole process, L-Borneol extraction rate reached is to more than 90%, and the rate of recovery reaches more than 80%; Process for extracting, separating and purifying is simple, and extract fully, efficiency is high, loses little, and treatment capacity is large, is applicable to suitability for industrialized production.Below by accompanying drawing and example, technical scheme of the present invention is described in further detail.
Accompanying drawing explanation
Figure is the process flow sheet of extraction separation and purification L-Borneol of the present invention
Embodiment
Below provide embodiment, the present invention will be further described.
Embodiment one:
The extraction separation and purification method of a kind of L-Borneol of the present invention, adopts following processing step:
1, Simultaneous distillation-extraction: Herba Blumeae Balsamiferae leaf and spray are pulverized for Herba Blumeae Balsamiferae powder-material, granularity is 0.1 ~ 1mm, Herba Blumeae Balsamiferae powder-material 50g after pulverizing adds in 1L water, be heated to micro-generation water vapor that boils, heat micro-the boiling of 100mL sherwood oil simultaneously and produce sherwood oil steam, the fat-soluble volatile component that when two-phase steam meets, sherwood oil steam extraction water vapor carries, both are condensation simultaneously in prolong, because water and the immiscible property of sherwood oil make both be separated, wherein distilling aqueous phase is back in water bottle, sherwood oil is back in sherwood oil bottle mutually, whole process is 5h, obtain Herba Blumeae Balsamiferae petroleum ether extract,
2, reduction vaporization: Herba Blumeae Balsamiferae petroleum ether extract is evaporated under reduced pressure atmosphere, pressure is 0.01MPa, temperature is 25 DEG C, time is 0.5h, obtain L-Borneol crude product 0.5021g, GC detects L-Borneol content and reaches 50%, and extraction rate reached is to more than 90%, and evaporation obtains the raw material that sherwood oil can continue as Simultaneous distillation-extraction;
3, Decompression Sublimation: L-Borneol crude product is carried out Decompression Sublimation, pressure is 0.01MPa, and temperature is 50 DEG C, and the time is 2h, collects crystal in condenser and namely obtains L-Borneol 0.2116g, and GC detects and confirms that quality meets " Chinese Pharmacopoeia 2010 " requirement, and the rate of recovery reaches 80%.
The distillation related in this example, extraction, condensation, reduction vaporization, squeezing, Decompression Sublimation are common process.
Embodiment two:
The extraction separation and purification method of a kind of L-Borneol of the present invention, adopts following processing step:
1, Simultaneous distillation-extraction: Herba Blumeae Balsamiferae leaf and spray are pulverized for Herba Blumeae Balsamiferae powder-material, granularity is 0.1 ~ 1mm, Herba Blumeae Balsamiferae powder-material 5kg after pulverizing adds in 5L water, be heated to micro-generation water vapor that boils, heat micro-the boiling of 1L sherwood oil simultaneously and produce sherwood oil steam, the fat-soluble volatile component that when two-phase steam meets, sherwood oil steam extraction water vapor carries, both are condensation simultaneously in prolong, because water and the immiscible property of sherwood oil make both be separated, wherein distilling aqueous phase is back in water bottle, sherwood oil is back in sherwood oil bottle mutually, whole process is 10h, obtain Herba Blumeae Balsamiferae petroleum ether extract,
2, reduction vaporization: Herba Blumeae Balsamiferae petroleum ether extract is evaporated under reduced pressure atmosphere, pressure is 0.05MPa, temperature is 30 DEG C, time is 2h, obtain L-Borneol crude product 48.7g, GC detects L-Borneol content and reaches 52%, and extraction rate reached is to more than 90%, and evaporation is collected sherwood oil and can be continued as Simultaneous distillation-extraction raw material;
3, Decompression Sublimation: L-Borneol crude product is carried out Decompression Sublimation, pressure is 0.09MPa, and temperature is 150 DEG C, time is 10h, collect crystal in condenser and namely obtain L-Borneol 22.7g, GC detects and confirms that quality meets " Chinese Pharmacopoeia 2010 " requirement, and the rate of recovery reaches more than 80%.
Embodiment three:
The extraction separation and purification method of a kind of L-Borneol of the present invention, adopts following processing step:
1, Simultaneous distillation-extraction: Herba Blumeae Balsamiferae leaf and spray are pulverized for Herba Blumeae Balsamiferae powder-material, granularity is 0.1 ~ 1mm, Herba Blumeae Balsamiferae powder-material 10kg after pulverizing adds in 10L water, be heated to micro-generation water vapor that boils, heat micro-the boiling of 1L sherwood oil simultaneously and produce sherwood oil steam, the fat-soluble volatile component that when two-phase steam meets, sherwood oil steam extraction water vapor carries, both are condensation simultaneously in prolong, because water and the immiscible property of sherwood oil make both be separated, wherein distilling aqueous phase is back in water bottle, sherwood oil is back in sherwood oil bottle mutually, whole process is 10h, obtain Herba Blumeae Balsamiferae petroleum ether extract,
2, reduction vaporization: Herba Blumeae Balsamiferae petroleum ether extract is evaporated under reduced pressure atmosphere, pressure is 0.02MPa, and temperature is 30 DEG C, and the time is 5h, obtains L-Borneol crude product 96.3g, and GC detects L-Borneol content and reaches 50%, and extraction rate reached is to more than 90%; Evaporation is collected sherwood oil and can be continued as Simultaneous distillation-extraction raw material;
3, Decompression Sublimation: L-Borneol crude product is carried out Decompression Sublimation, pressure is 0.05MPa, and temperature is 100 DEG C, time is 10h, collect crystal in condenser and namely obtain L-Borneol 39.7g, GC detects and confirms that quality meets " Chinese Pharmacopoeia 2010 " requirement, and the rate of recovery reaches more than 80%.
Claims (2)
1. an extraction separation and purification method for L-Borneol, is characterized in that adopting following processing step:
(1) raw material: get Herba Blumeae Balsamiferae leaf and spray is that raw material is pulverized, grinding particle size is 0.1 ~ 1mm;
(2) Simultaneous distillation-extraction: the Herba Blumeae Balsamiferae powder-material after pulverizing is added to the water, be heated to micro-generation water vapor that boils, micro-the boiling of heat oil ether produces sherwood oil steam simultaneously, the fat-soluble volatile component that when two-phase steam meets, sherwood oil steam extraction water vapor carries, both are condensation simultaneously in prolong, because water and the immiscible property of sherwood oil make both be separated, obtain Herba Blumeae Balsamiferae petroleum ether extract, whole process is 5 ~ 10h;
(3) reduction vaporization: previous step is obtained Herba Blumeae Balsamiferae petroleum ether extract and evaporate under reduced pressure atmosphere, pressure is 0.01 ~ 0.09MPa, and temperature is 10 ~ 30 DEG C, and the time is 0.5 ~ 2h, obtains L-Borneol crude product;
(4) Decompression Sublimation: L-Borneol crude product obtained in the previous step is carried out Decompression Sublimation, pressure is 0.01 ~ 0.09MPa, and temperature is 50 ~ 150 DEG C, and the time is 1 ~ 10h, collects crystal in condenser and namely obtains L-Borneol.
2. the extraction separation and purification method of a kind of L-Borneol according to claim 1, it is characterized in that described Herba Blumeae Balsamiferae is composite family Herba Blumeae Balsamiferae platymiscium Herba Blumeae Balsamiferae (Latin is called Blumeabalsamifera (L.) DC.), originate in Luodian County, Guizhou Province.
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Families Citing this family (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104030888B (en) * | 2014-06-03 | 2015-12-09 | 江口县苗药生物科技有限公司 | A kind of high purity L-Borneol extraction element |
| 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 |
| CN109134193A (en) * | 2017-06-27 | 2019-01-04 | 贵州艾源生态药业开发有限公司 | A kind of method that Blumea balsamifera extracts borneol |
| CN109134194A (en) * | 2017-06-28 | 2019-01-04 | 贵州省罗甸县全兴药业开发有限责任公司 | A kind of Blumea balsamifera extracts the manufacture craft of borneol |
| CN109212043A (en) * | 2017-07-01 | 2019-01-15 | 贵州艾源生态药业开发有限公司 | The measuring method of content of bornyl alcohol in a kind of Blumea balsamifera |
| CN109971547A (en) * | 2019-04-28 | 2019-07-05 | 中国农业科学院烟草研究所 | A method of utilizing deep congruent melting solvent extraction wormwood essential oil |
| CN110101730B (en) * | 2019-06-10 | 2021-07-23 | 贵州艾力康中草药开发有限公司 | Processing method for preventing reduction of active ingredients of blumea balsamifera |
| CN110075149B (en) * | 2019-06-10 | 2021-07-23 | 贵州艾力康中草药开发有限公司 | Blumea balsamifera extract and preparation method thereof |
| CN110658283B (en) * | 2019-11-14 | 2022-11-01 | 天津中医药大学 | Method for detecting volatile components of folium artemisiae argyi |
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| CN101735050A (en) * | 2010-01-21 | 2010-06-16 | 上海交通大学 | Blumeabalsamifera extract as well as extracting method and application thereof |
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| GB2052974A (en) * | 1979-05-11 | 1981-02-04 | Yin Chen | Essential oils |
| CN201334471Y (en) * | 2009-01-21 | 2009-10-28 | 中国热带农业科学院热带作物品种资源研究所 | Blumea balsamifera powder extracting device |
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