CN108042758A - A kind of method that volatile oil in curcuma zedoary medicinal material is separated based on postcritical preparative - Google Patents
A kind of method that volatile oil in curcuma zedoary medicinal material is separated based on postcritical preparative Download PDFInfo
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- CN108042758A CN108042758A CN201711407197.0A CN201711407197A CN108042758A CN 108042758 A CN108042758 A CN 108042758A CN 201711407197 A CN201711407197 A CN 201711407197A CN 108042758 A CN108042758 A CN 108042758A
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K36/00—Medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicines
- A61K36/18—Magnoliophyta (angiosperms)
- A61K36/88—Liliopsida (monocotyledons)
- A61K36/906—Zingiberaceae (Ginger family)
- A61K36/9066—Curcuma, e.g. common turmeric, East Indian arrowroot or mango ginger
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D11/00—Solvent extraction
- B01D11/02—Solvent extraction of solids
- B01D11/0203—Solvent extraction of solids with a supercritical fluid
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2236/00—Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
- A61K2236/30—Extraction of the material
- A61K2236/37—Extraction at elevated pressure or temperature, e.g. pressurized solvent extraction [PSE], supercritical carbon dioxide extraction or subcritical water extraction
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Abstract
The invention discloses a kind of method of volatile oil in preparative separation curcuma zedoary medicinal material based on means of supercritical extraction, the method, step is as follows：Curcuma zedoary pulverizing medicinal materials are fitted into supercritical extraction reactor, and heating extraction, extraction temperature is 30 50 DEG C, 10 30MPa of CO2 Fluid pressures, 10 25L.h of CO2 flows‑1, 1 3h of extraction time, collection product, method of the invention, product yield and purity increase compared with existing process, and reproducible, easy to operate quick, safe, energy-saving and emission-reduction, suitable for industrialized production.
Description
Technical field
The present invention relates to the efficient preparative separation technologies of curcuma zedoary, and in particular to one kind separates cowherb based on postcritical preparative
The method of volatile oil in art medicinal material.
Background technology
Curcuma zedoary is a kind of dry rhizome of zingiberaceous plant zedoary, Guangxi zedoary or Curcuma wenyujin.Traditional Chinese medical theory thinks, cowherb
Art has the effect of promoting the circulation of qi blood-breaking, Xiao Ji Zhi Tong.Mainly containing volatile oil component in curcuma zedoary, the main composition of volatile oil is a variety of sesquialters
Triterpene derivative and eucalyptol, wherein curdione content are about 1%-2.5%.Germacrone and curdione have apparent anti-swollen
Knurl physiological activity.Beta-elemene is the effective monomer extracted from Chinese medicine Curcuma wenyujin rhizome, is the antitumor 3 kinds of active ingredient of elemene
One of.Extensive with antitumor spectra, curative for effect, adverse reaction is slight, and it is excellent to significantly improve the protrusion such as Quality of Life of Patients with Tumor
Point.Modern study confirms that Curcuma Aromatic Oil has promoting the circulation of qi blood-breaking, Xiao Ji Zhi Tong, anti-inflammatory, antiviral, antitumor, the immune work(of enhancing
The effects that energy and inhibition thrombosis.
Following Chinese patent discloses the preparation method of Curcuma Aromatic Oil：
200410064570.3 supercritical CO2The method of elemene in fluid extraction-rectification extraction curcuma zedoary
A kind of 200910177025.8 method of the extraction separation curdione from oil of zedoary turmeric
200410059643.X the extraction process of rcumenol
201210560585.3 a kind of method of volatile oil extracting and its comprehensive utilization of cellulose in Chinese herbal medicine
But preparation condition in above-mentioned patent is harsh, and in curcuma zedoary volatile oil recovery rate it is low, cause the wasting of resources.
The content of the invention
The technical problems to be solved by the invention be to provide that a kind of extracting method is simple, yield is high and purity it is higher based on
The method of volatile oil in the preparative separation curcuma zedoary medicinal material of means of supercritical extraction.
Technical solution is used by the present invention solves above-mentioned technical problem：A kind of preparative based on means of supercritical extraction point
Method from volatile oil in curcuma zedoary medicinal material, its step are as follows：
A curcuma zedoary pulverizing medicinal materials are mixed with bead to be fitted into supercritical extraction reactor, and heating extraction, storage tank is cooled down；
B extraction conditions therein is as follows：Extraction temperature is 30-50 DEG C, CO2Fluid pressure 10-30MPa, CO2Flow 10-
25L/h-1, extraction time 1-3h.
C purifies curdione, germacrone, elemene by rectifying column respectively, collects each product.
Preferably extraction conditions is：Using extraction temperature as 50 DEG C, CO2Fluid pressure 10MPa, CO2Flow 10L.h-1, extraction
Rectifying time 3h, obtains volatile oil.
The present invention provides a kind of methods that volatile oil in curcuma zedoary medicinal material is separated based on postcritical preparative, add cowherb
The recovery rate of volatile oil in art, the utilization rate of medicinal material of raising avoid the wasting of resources, while use supercritical CO2Extraction
Method, overcoming conventional organic solvents extraction method, time-consuming, the problems such as such as using toxic solvent and dissolvent residual.
The extraction conditions of the present invention is obtained by screening, compared to the prior art, is had the following advantages：
1. using means of supercritical extraction technology extraction Curcuma Aromatic Oil, overcoming conventional organic solvents extraction method, time-consuming, toxic molten
The problems such as agent and dissolvent residual.
2. curdione, germacrone, elemene are extracted respectively using the rectifying column separation of means of supercritical extraction.
3. during using means of supercritical extraction technology extraction Curcuma Aromatic Oil, curcuma zedoary medicinal material is smashed and is mixed with bead, is effectively improved
Extraction efficiency, the problem of easily caking when preventing fresh curcuma zedoary from extracting.
The extraction conditions of the present invention, screening process are as follows：
Being crushed after cutting using fresh curcuma zedoary respectively for the present invention is extraction raw material, after extraction raw material is sufficiently mixed with bead
It is fitted into supercritical extraction reactor and is extracted, extraction conditions screening is as follows：
By the comparison of recovery rate, extraction process is using Extracting temperature as major influence factors, and CO2 Fluid pressures are, CO2Flow is
Minor effect filters out said extracted extraction conditions.
The present invention with the extraction of rectifying column, extracts curdione, germacrone, elemene, because three's polarity has one respectively simultaneously
It is fixed to distinguish, in CO2Dissolubility is different in fluid, is adjusted by pressure and temperature and carries out rectifying, after pressure is more than 10MPa, leads to
Excess temperature adjusts stage extraction and carries out component separation, wherein 1 section 40 DEG C of rectifying, 2 sections 45 DEG C of rectifying, 3 sections 55 DEG C of rectifying, rectifying 2
65 DEG C of section, difference Extraction and enrichment curdione, germacrone, elemene,.
Specific embodiment
The present invention is described in further detail with reference to embodiments.
Embodiment 1
Curcuma zedoary medicinal material is extracted into raw material through crushing, extraction raw material is fitted into supercritical extraction reactor.Separating still is carried out
Heating, storage tank are cooled down.It is 30 DEG C in extraction temperature, CO2Fluid pressure 10MPa, CO2Flow 10L.h-1, extraction time 1h
Under the conditions of, obtain the extractive of volatile oil of yellowish-brown oily extracted in curcuma zedoary medicinal material.The volatile oil yield of the extract
4.63%, wherein curdione content 2.481%, germacrone content are 0.124%, and beta-elemene content is 0.0118%.
Embodiment 2
Substantially the same manner as Example 1, different is simply 30-50 DEG C, CO2 Fluid pressure 20MPa in extraction temperature,
CO2 flows 18L.h-1, extract is obtained under the conditions of extraction time 2h.The volatile oil yield 3.04% of the extract, wherein curcuma zedoary
Diketone content 1.652%, germacrone content are 0.242%, and beta-elemene content is 0.0231%.
Embodiment 3
Substantially the same manner as Example 1, different is simply 30 DEG C in extraction temperature, CO2 Fluid pressures 30MPa, CO2 stream
Measure 25L.h-1, extract is obtained under the conditions of extraction time 3h.The volatile oil yield 3.04% of the extract, wherein curdione contain
Amount 1.512%, germacrone content are 0.216%, and beta-elemene content is 0.0207%.
Embodiment 4
Substantially the same manner as Example 1, different is simply 40 DEG C in extraction temperature, CO2 Fluid pressures 10MPa, CO2 stream
Measure 18L.h-1, extract is obtained under the conditions of extraction time 3h.The volatile oil yield 3.92% of the extract, wherein curdione contain
Amount 2.125%, germacrone content are 0.257%, and beta-elemene content is 0.0243%.
Embodiment 5
Substantially the same manner as Example 1, different is simply 40 DEG C in extraction temperature, CO2 Fluid pressures 20MPa, CO2 stream
Measure 25L.h-1, extract is obtained under the conditions of extraction time 1h.The volatile oil yield 1.82% of the extract, wherein curdione contain
Amount 1.025%, germacrone content are 0.0101%, and beta-elemene content is 0.0094%.
Embodiment 6
Substantially the same manner as Example 1, different is simply 40 DEG C in extraction temperature, CO2 Fluid pressures 30MPa, CO2 stream
Measure 10L.h-1, extract is obtained under the conditions of extraction time 2h.The volatile oil yield 2.56% of the extract, wherein curdione contain
Amount 1.441%, germacrone content are 0.162%, and beta-elemene content is 0.0151%.
Embodiment 7
Substantially the same manner as Example 1, different is simply 50 DEG C in extraction temperature, CO2 Fluid pressures 10MPa, CO2 stream
Measure 25L.h-1, extract is obtained under the conditions of extraction time 2h.The volatile oil yield 3.52% of the extract, wherein curdione contain
Amount 1.95%, germacrone content are 0.186%, and beta-elemene content is 0.018%.
Embodiment 8
Substantially the same manner as Example 1, different is simply 50 DEG C in extraction temperature, CO2 Fluid pressures 20MPa, CO2 stream
Measure 10L.h-1, extract is obtained under the conditions of extraction time 3h.The volatile oil yield 4.16% of the extract, wherein curdione contain
Amount 2.231%, germacrone content are 0.229%, and beta-elemene content is 0.0233%.
Embodiment 9
Substantially the same manner as Example 1, different is simply 50 DEG C in extraction temperature, CO2 Fluid pressures 30MPa, CO2 stream
18L.h-1 is measured, extract is obtained under the conditions of extraction time 1h.The volatile oil yield 3.68% of the extract, wherein curdione
Content 2.036%, germacrone content are 0.241%, and beta-elemene content is 0.0237%.
Above-mentioned curcuma zedoary medicinal material extract volatile oil be according to【Assay】It is measured according to high performance liquid chromatography (general rule 0512),
Japanese Shimadzu LC-20AT types high performance liquid chromatograph (SIL-20A autosamplers, CTO-10AS column ovens, SPD-M20A detections
Device)；Labsolutions work stations, chromatographic condition Waters symmetry C18 chromatographic columns (4.6mm × 250mm, 5 μm), stream
Dynamic phase acetonitrile-water (60: 40), Detection wavelength 210nm, 35 DEG C of column temperature, flow velocity 1.0mLmin-1., content is calculated according to result：
The above results are obtained a result using oil yield as index through Mathematical Statistics Analysis：Using extraction temperature as 50 DEG C, CO2 streams
Body pressure 10MPa, CO2 flow 10L.h-1, extraction time 3h.Cowherb is separated based on postcritical preparative the present invention provides one kind
The method of volatile oil in art medicinal material, add the recovery rate of volatile oil in curcuma zedoary, and the utilization rate of medicinal material of raising avoids money
Source wastes, while using supercritical carbon dioxide fluid extraction, overcoming conventional organic solvents extraction method, time-consuming, such as to use toxic molten
The problems such as agent and dissolvent residual.
Claims (3)
1. a kind of method of volatile oil in preparative separation curcuma zedoary medicinal material based on means of supercritical extraction, it is characterised in that：It is by
Curcuma zedoary medicinal material extracts volatile oil for raw material, it is characterized in that：Comprise the following steps：
A, curcuma zedoary pulverizing medicinal materials are taken, cross 30 mesh sieves, to extract raw material,
B, raw material is mixed to be fitted into supercritical extraction reactor with bead and is extracted, volatile oil is prepared, wherein described overcritical
CO2The condition of extraction is：Extraction temperature is 30-50 DEG C, CO2Fluid pressure 10-30MPa, CO2Flow 10-25L.h-1, during extraction
Between 1~3h；
Wherein, volatile oil yield is 2.98%-4.63%, and wherein curdione content is 1.025%-2.481%；Germacrone contains
It measures as 0.0101%-0.257%, beta-elemene content is 0.0094%-0.0243%.
2. the method as described in claim 1, it is characterized in that：The supercritical CO2The condition of extraction is：Using extraction temperature as 50
DEG C, CO2 Fluid pressures 10MPa, CO2Flow 10L.h-1, extraction time 3h, volatile oil yield 4.63%, wherein curdione contain
Amount 2.481%, germacrone content are 0.124%, and beta-elemene content is 0.0118%.
3. the method as described in claim 1, it is characterized in that curcuma zedoary medicinal material is the dry root of zedoary, Guangxi zedoary or Curcuma wenyujin
Stem.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109232214A (en) * | 2018-09-20 | 2019-01-18 | 无锡济民可信山禾药业股份有限公司 | The feeding method of Moschus in a kind of Moschus extraction process |
| CN109381680A (en) * | 2019-01-03 | 2019-02-26 | 西藏未来生物医药有限公司 | A kind of preparation method of curcuma zedoary oil spray |
| CN109456830A (en) * | 2018-11-27 | 2019-03-12 | 河南羚锐制药股份有限公司 | The supercritical extraction method of volatile oil in a kind of activating meridians to stop pain plaster material |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109232214A (en) * | 2018-09-20 | 2019-01-18 | 无锡济民可信山禾药业股份有限公司 | The feeding method of Moschus in a kind of Moschus extraction process |
| CN109456830A (en) * | 2018-11-27 | 2019-03-12 | 河南羚锐制药股份有限公司 | The supercritical extraction method of volatile oil in a kind of activating meridians to stop pain plaster material |
| CN109381680A (en) * | 2019-01-03 | 2019-02-26 | 西藏未来生物医药有限公司 | A kind of preparation method of curcuma zedoary oil spray |
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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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