CN108276248A - A method of based on borneol in postcritical preparative separating borneol camphor tree branches and leaves - Google Patents
A method of based on borneol in postcritical preparative separating borneol camphor tree branches and leaves Download PDFInfo
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- CN108276248A CN108276248A CN201711407196.6A CN201711407196A CN108276248A CN 108276248 A CN108276248 A CN 108276248A CN 201711407196 A CN201711407196 A CN 201711407196A CN 108276248 A CN108276248 A CN 108276248A
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- borneol
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- leaves
- extract
- camphor tree
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C29/00—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring
- C07C29/74—Separation; Purification; Use of additives, e.g. for stabilisation
- C07C29/76—Separation; Purification; Use of additives, e.g. for stabilisation by physical treatment
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/50—Improvements relating to the production of bulk chemicals
- Y02P20/54—Improvements relating to the production of bulk chemicals using solvents, e.g. supercritical solvents or ionic liquids
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- Organic Chemistry (AREA)
- Medicines Containing Plant Substances (AREA)
- Acyclic And Carbocyclic Compounds In Medicinal Compositions (AREA)
Abstract
The invention discloses it is a kind of from borneol camphor tree branches and leaves extract borneol method, the method, including：The fresh branches and leaves of borneol camphor tree extract raw material through crushing, and extraction raw material is fitted into supercritical extraction reactor and is sufficiently mixed extraction with bead.Extraction temperature is 32 42 DEG C, 8 11MPa of CO2 Fluid pressures, 10 25L.h 1 of CO2 flows, 15~30min of extraction time, extract crystallisation by cooling obtain borneol crystal, the present invention research shows that, by the method for supercritical extract, product yield and purity increase compared with prior art, and reproducible, it is easy to operate quick, safe, energy-saving and emission-reduction are suitable for industrialized production.
Description
Technical field
The present invention relates to the efficient preparative separation technologies of borneol, and in particular to one kind is based on postcritical preparative separation dragon
The method of borneol in the fresh branches and leaves of brain camphor tree.
Background technology
The plant origin of natural borneol mainly has borneol camphor tree in cinnamomum camphora, borneol type plant and the Borneolum tree three of burmannii in oily camphor tree
Kind canella.Though it is (i.e. cinnamomum camphora, oily camphor tree, burmannii) not of the same race that three kinds of canellas belong to Lauraceae, chemical type is borneol
Type.Borneol camphor tree is that Lauraceae hits a specific chemicals type plant for belonging to and being rich in d-Bomeol (natural borneol) in cinnamomum camphora tree, at me
Best source of the state as extraction natural borneol, and the volatile oil of leaf is based on borneol.The ingredient of borneol camphor tree volatile oil mainly may be used
It is divided into monoterpenes, sesquiterpenoids, oxygen-containing terpene etc., wherein for d-Bomeol content above, oxygen-containing terpene is that borneol camphor tree is planted in oil
The most chemical composition of object content.Borneol Central nervous excitability has dual regulation, can be " tranquilizing and allaying excitement " and awake
Brain acts on；It can also promote drug to penetrate blood-brain barrier, improve some drugs vivo biodistribution availability and blood concentration；Also have
There is the effects that antibacterial, anti-inflammatory, analgesic activity.
Invention content
The simple, rate of recovery that technical problem to be solved by the invention is to provide a kind of extracting methods and purity is higher is based on
The method of borneol in the imperial camphor tree branches and leaves of preparative separation of means of supercritical extraction.
Technical solution is used by the present invention solves above-mentioned technical problem：A kind of side extracting borneol from borneol camphor tree branches and leaves
Method, its step are as follows：
The fresh branches and leaves of borneol camphor tree through crushing as extraction raw material, extraction raw material are fitted into supercritical extraction reactor and bead by a
It is sufficiently mixed；
The condition of supercritical extract described in b is that extraction temperature is 32~42 DEG C, CO2 Fluid pressures 8~11MPa, CO2 flow 10
Under~25L.h-1,15~30min of extraction time.
C collects extract liquor, and crystallisation by cooling is to get borneol.
Preferably the condition of supercritical extract is：38 DEG C of temperature, CO2 Fluid pressures 10MPa, CO2 flow 10L.h-1, when extraction
Between 20min, obtain extract.
The preparative based on means of supercritical extraction that compared with the prior art, the advantages of the present invention are as follows a kind of detaching imperial branck of Lignum cinnamomi camphorae
The method of borneol in leaf, the fresh branches and leaves of borneol camphor tree through crush for extraction raw material, will extraction raw material is fitted into supercritical extraction reactor and
Bead is sufficiently mixed extraction.Extraction temperature is 32~42 DEG C, CO2 Fluid pressures 8~11MPa, CO2 10~25L.h-1 of flow,
Extraction time 15-30min, extract crystallisation by cooling obtain borneol crystal.This method is prepared simply, and borneol recovery rate is about
80%, purity is about 71%.
The extracting process of the present invention is obtained by screening, and screening process is as follows：
The present invention's uses the fresh branches and leaves of borneol camphor tree through crushing as extraction raw material respectively, by borneol camphor tree fresh branches and leaves extraction raw material with
Bead is fitted into supercritical extraction reactor after being sufficiently mixed and is extracted, and extraction conditions screening is as follows：
By the comparison of recovery rate, extraction process is with CO2Fluid pressure is major influence factors, CO2Flow is minor effect, sieve
Select above-mentioned optimal extraction extraction conditions as above [0005] item.
It is as follows that the extracting process and the prior art of the present invention compares advantage：
Specific implementation mode
Present invention is further described in detail with reference to embodiments.
Embodiment 1
By the fresh branches and leaves of borneol camphor tree through crushing as extraction raw material, weigh 500g, is fitted into supercritical extraction reactor and glass
Pearl is sufficiently mixed.Under the conditions of extracting pressure 8MPa, 32 DEG C of temperature, CO2 flows 10L.h-1, time 15min, borneol camphor tree is obtained
The translucent crystalloid Borneolum Syntheticum extract extracted in fresh branches and leaves.The purity 67.23% of the extract, recovery rate 75.27%.
Embodiment 2
It is substantially the same manner as Example 1, it is different only extracting pressure 9MPa, temperature 45 C, CO2 flows 20L.h-1,
Extract is obtained under the conditions of time 20min.The purity 65.28% of the extract, recovery rate 77.42%.
Embodiment 3
Substantially the same manner as Example 1, different is in extracting pressure 10MPa, 38 DEG C of temperature, CO2 flows 20L.h-
1, extract is obtained under the conditions of time 25min.The purity 68.41% of the extract, recovery rate 71.23%.
Embodiment 4
Substantially the same manner as Example 1, different is in extracting pressure 11MPa, 38 DEG C of temperature, CO2 flows 15L.h-
1, extract is obtained under the conditions of time 30min.The purity 65.12% of the extract, recovery rate 80.23%.
Embodiment 5
It is substantially the same manner as Example 1, it is different only extracting pressure 9MPa, 41 DEG C of temperature, CO2 flows 20L.h-1,
Extract is obtained under the conditions of time 20min.The purity 70.82% of the extract, recovery rate 68.85%.
Embodiment 6
Substantially the same manner as Example 1, different is in extracting pressure 10MPa, 38 DEG C of temperature, CO2 flows 20L.h-
1, extract is obtained under the conditions of time 25min.The purity 72.41% of the extract, recovery rate 76.11%.
Embodiment 7
Substantially the same manner as Example 1, different is in extracting pressure 10MPa, 38 DEG C of temperature, CO2 flows 10L.h-
1, extract is obtained under the conditions of time 20min.The purity 71.18% of the extract, recovery rate 80.44%.
The purity detecting of borneol is according to 2015 editions in above-mentioned borneol camphor tree branches and leaves extract《Chinese Pharmacopoeia》Gas chromatography
(general rule 0521) measures.Chromatographic condition：DB-5 chromatographic columns (30m250mm0.25 μm)；Ammonia flame ionic detector (FID),
300 DEG C of temperature；Carrier gas, N2；300 DEG C of injector temperature；0.5 μ l of sample size.Temperature programming：Column temperature:80 DEG C, 2min is kept the temperature, with 3
DEG C/min rises to 150 DEG C, according to as a result, calculating natural borneol purity.The calculation formula of natural borneol yield θ is：
Wherein：M1-crystallized product quality
Borneol quality in borneol camphor tree branches and leaves before m2-extraction
The present invention preferably improves the product yield and purity of borneol, and easy to operate quick, safe, energy saving to subtract
Row is suitable for industrialized production.
Claims (4)
1. a kind of method for extracting borneol from borneol camphor tree branches and leaves, it is characterised in that：Steps are as follows：The fresh branches and leaves of borneol camphor tree are through crushing
As extraction raw material, extraction raw material is fitted into after being sufficiently mixed with bead in supercritical extraction reactor and is extracted, collect extract liquor, it is cold
But it crystallizes to get borneol.
2. according to the method described in claim 1, it is characterized in that：The condition of the supercritical extract is：32~42 DEG C of temperature,
CO2 Fluid pressures 8~11MPa, CO2 10~25L.h-1 of flow, 15~30min of extraction time.
3. according to the method described in claim 1, it is characterized in that：The condition of the supercritical extract is：38 DEG C of temperature, CO2
Fluid pressure 10MPa, CO2 flow 10L.h-1, extraction time 20min.
4. according to the method described in claim 1, it is characterized in that：The borneol raw material are crushed by the fresh branches and leaves of borneol camphor tree
Gained.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201711407196.6A CN108276248A (en) | 2017-12-22 | 2017-12-22 | A method of based on borneol in postcritical preparative separating borneol camphor tree branches and leaves |
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| CN201711407196.6A CN108276248A (en) | 2017-12-22 | 2017-12-22 | A method of based on borneol in postcritical preparative separating borneol camphor tree branches and leaves |
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| CN108276248A true CN108276248A (en) | 2018-07-13 |
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| CN201711407196.6A Pending CN108276248A (en) | 2017-12-22 | 2017-12-22 | A method of based on borneol in postcritical preparative separating borneol camphor tree branches and leaves |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109913318A (en) * | 2019-04-10 | 2019-06-21 | 范加家 | A kind of supercritical extraction method of borneol essential oil |
| CN110003982A (en) * | 2019-04-10 | 2019-07-12 | 范加家 | A kind of combined type borneol method of extraction of essential oil |
| CN115611837A (en) * | 2022-12-15 | 2023-01-17 | 江西省科学院应用化学研究所 | Sesquiterpene lactone derivative and preparation method thereof |
-
2017
- 2017-12-22 CN CN201711407196.6A patent/CN108276248A/en active Pending
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109913318A (en) * | 2019-04-10 | 2019-06-21 | 范加家 | A kind of supercritical extraction method of borneol essential oil |
| CN110003982A (en) * | 2019-04-10 | 2019-07-12 | 范加家 | A kind of combined type borneol method of extraction of essential oil |
| CN115611837A (en) * | 2022-12-15 | 2023-01-17 | 江西省科学院应用化学研究所 | Sesquiterpene lactone derivative and preparation method thereof |
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| CB02 | Change of applicant information |
Address after: 214028 Changjiang South Road, new Wu District, Wuxi, Jiangsu Province, No. 12 Applicant after: Wuxi Jiyu Shanhe Pharmaceutical Co., Ltd Applicant after: JINGXI JIMIN KEXIN GROUP Co.,Ltd. Address before: 214028 No. 12 Changjiang South Road, New District, Jiangsu, Wuxi Applicant before: WUXI JIMIN KEXIN SHANHE PHARMACEUTICAL Co.,Ltd. Applicant before: JINGXI JIMIN KEXIN GROUP Co.,Ltd. |
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Application publication date: 20180713 |
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