CN107412292A - The method that general flavone and volatile oil are produced using malabar nut - Google Patents
The method that general flavone and volatile oil are produced using malabar nut Download PDFInfo
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- 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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- A61K2236/50—Methods involving additional extraction steps
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- A61K2236/55—Liquid-liquid separation; Phase separation
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Abstract
A kind of method that adhatodine and volatile oil can be synchronously extracted from malabar nut present invention aim to provide method：Malabar nut cauline leaf after dried is through supercritical CO2After extraction, the yield about 1.5% of volatile oil.Residue after extraction after microbial fermentation, then extracted with ethanol, filter, be concentrated under reduced pressure, the adhatodine sterling that purity is more than 95% is made in adsorpting column chromatography, ion-exchange chromatography, crystallization of decolourizing.Operating condition of the present invention is simple, and extraction efficiency is high.
Description
Technical field
The invention belongs to natural products manufacture field, is related to a kind of side that general flavone and volatile oil are produced from malabar nut
Method.
Background technology
Malabar nut is called Paraboea dictyoneura (Hance) B. L (Burtt), refutes bone, large osteosynthesis etc. greatly, is Acanthaceae Adhatoda Nees evergreen shrubs, is distributed mainly on
The Asia southeast, there are production, or cultivation on China Guangdong, Guangxi, Hainan, Macao, Hong Kong, Yunnan and other places, or it is wild.The plant master
It is characterized in：Big shrub, up to 1-3 rice；Cylindric, the grey of branch, there is a hole skin, and spray is close by the micro- pubescence of canescence.Leaf papery, square
Round shape lanceolar is avette to lanceolar, or avette or ellipticity, long 15-20 centimetres, and wide 4.5-7.5 centimetres, top is tapering, sometimes
Slightly be in shape of tail, base portion wealthy wedge shape, full edge, above it is near hairless, the back side is by micro- pubescence；Middle arteries are on upper mask slot, the every side about 12 of lateral vein
Bar；Petiole is long 1.5-2 centimetres.Cauline leaf has special foul smell after rubbing.Spike is avette or slightly extends；Bennet is long 5-10 centimetres；Bud
Piece is avette or wealthy avette, long 1-3 centimetres, wide 8-15 millimeters, by micro- pubescence；Squamella lanceolar, slightly shorter than bract, calyx lobe 5,
Square round shape lanceolar, is about 8 millimeters；Corolla white, there is purple fringe or pink, long 2.5-3 centimetres, by pubescence, is preced with pipe ovum
Shape, it is about 6 millimeters；Coyote hole ellipse, base portion generally have ball attachment thing unobvious.Capsule is closely wooden, is about 0.5 centimetre, on
Portion has 4 seeds, the solid short handle shape in bottom.
Malabar nut is traditional Chinese medicine, complete stool segment, dries or using fresh herb is used as medicine, is the ground prescription that South China of China uses
Material refutes greatly traditional the Dai nationality medicine in the area such as bone, and Xishuangbanna of Yunnan province.The traditional Chinese medical science thinks its acrid flavour, slight bitter, mild-natured, returns
Liver, the spleen channel；There are expelling wind and activating blood flow, blood stasis removing analgesic, the continuous wound of synthetism and other effects.Clinically cure mainly muscles and bones to traumatic fracture, sprain, extravasated blood swelling and pain,
Bi condition, pain in the back, menorrhalgia, uterine bleeding, for oral administration or external application.
Malabar nut chemical composition mainly contains alkaloids and flavone compound, also containing a variety of glycosides and polysaccharide
Compound and volatile oil component.
Flavone compound has extensive physiologically active and pharmacological action, such as anti-oxidant, anti-aging, antitumor, drop blood
Fat, radioresistance, anti-inflammatory myogenic, improve the multinomial physiological function such as immune.Flavones ingredient includes Kaempferol, quercitrin in malabar nut
Element, 2- hydroxyls -4- glucosyloxies chalcone and Vitexin, isovitexin, 2 "-O- xylosylvitexins, 5,7,4 '-three hydroxyls
(base) flavones.
Flavone compound is typically all dissolved in methanol, ethanol polar solvent, and it is organic to be insoluble in benzene, chloroform, petroleum ether etc.
Solvent, and the dissolubility in water is then relevant with the hydroxyl introduced on parent nucleus.
The volatile oil of duckbilled floral leaf, flower and root extraction is a kind of with antibacterial, the spices of antiphlogistic activity, such as treating tuberculosis bar
Bacterium acts on, and the inhibition concentration to Mycobacterium hominis (B19-4) is 2g/mL, to ox type (B 19-3) or bird type (B19-1) tulase
It can be completely inhibited in 5g/mL.
At present, extract flavones respectively from plant and the research of volatile oil is very more, but the method about synchronously extracting
Report less, its method is essentially all using extraction by steam distillation, is then separated again with the method for distillation, resin
(CN106377582A, CN102106918A, CN105999022A, CN102671017A, CN104178350A,
CN103451022A, CN105362311A)
And considerably less , Sun Yun (2013) of research of volatile oil etc. is extracted from malabar nut and analyzes malabar nut Chinese medicine with GC-MS
With in the research of volatile oil and using extraction by steam distillation volatile oil.General flavone and volatilization are extracted from malabar nut simultaneously
The research of oil then has no report.
The present invention uses supercritical CO2Fluid extraction technology extracts volatile oil, and extracts general flavone from its residue, more
Plant resources effectively is utilized, is overcome in the traditional approach such as steam distillation, solvent reflux extraction and yield is present low (yield is not
To 0.2%), poor quality (color deep, smell miscellaneous), later separation is cumbersome the shortcomings of, consuming cost is relatively low, gained volatile oil purity
It is higher, technically there are steam distillation and the irreplaceable superiority of solvent method.
The content of the invention
Present invention aim to provide a kind of method to extract general flavone and volatile oil from malabar nut simultaneously
Method：Malabar nut cauline leaf after dried is through after crushed, passing through supercritical CO2Volatile oil is obtained by extraction；Residue after extraction
After microbial fermentation, then extracted with ethanol, filtered, general flavone is made in adsorption chromatography, decolouring, crystallization.
The microorganism fungus kind that the present invention uses, rough spore aspergillus (Aspergillus asperescens) are general from China
Logical Microbiological Culture Collection administrative center, numbering are respectively CGMCC No.3.4369.
It is characterized in that：
1st, malabar nut cauline leaf is gathered annual 8~October, dried, crushed, cross 20 mesh sieves.
2nd, the malabar nut stem and leaf powder to pulverize and sieve is added to supercritical CO2In the extraction kettle of extraction equipment, electricity is connected
Source, refrigeration switch is connected, control the circulating water temperature in ice chest then to be begun to warm up, extracting pressure 15 in the range of 0-5 DEG C
~30MPa, 35~55 DEG C of extraction temperature, 2~4h of extraction time, two 30~40 DEG C of separating still temperature, separating still pressure 8~
152MPa, fill factor 80%.After extraction, gained liquid, as duckbilled flowers volatile oil are released from separating still.
3rd, the freeze-dried rear addition rough spore aspergillus nutrient solutions of 5-10% of residue after extracting, it is aerobic solid under the conditions of 28~30 DEG C
Body ferments 3~5 days.
4th, the malabar nut after fermenting is at 20~40 DEG C, with the ethanol solution ultrasonic extraction 3 times of certain mass fraction, with pottery
Porcelain membrane filtration, 3 times filtrate merges.Filtrate obtains the crude extract of general flavone, and dried at 50 DEG C through ethanol is recovered under reduced pressure；
Dried object is extracted with chloroform, ceramic membrane filter obtains filter residue, and filtrate is concentrated under reduced pressure at 50 DEG C removes chloroform, and vacuum is done
It is dry.
5th, dried object is dissolved with a small amount of ethanol solution, and with ceramic membrane filter, filtrate is with D101 types or AB-8 type macroreticular resins
Purifying；Successively with deionized water, the ethanol elution of mass fraction 30%~90%, the as medicinal extract of collection ethanol phase, flavonoids
Compound crude extract.Recrystallized and dried with absolute ethyl alcohol after being concentrated under reduced pressure, it is dissolving crystallized with hot ethanol, add activated carbon to take off
Color, filtering, general flavone is obtained after freezing.
The filter process is all to use ceramic membrane filter, and fenestra pore size is 0.22 μm.
Technique effect
Hair method of the present invention has the following advantages that compared with existing conventional art：
1st, process of the invention is simple, and general flavone and volatile oil can be synchronously extracted from malabar nut, improves duckbilled
Colored utilization rate, it is quick to obtain various active composition；Technological process is also simplify simultaneously, advantageously reduces production cost；Prepare
Method is simple to operate, quick, efficient.
2nd, using CO2Supercritical technology extracts volatile oil, and technique is green, without any dissolvent residual, extraction time
Short, production cost is low, it is easy to accomplish industrialization.
3rd, in the environment of anaerobic and lucifuge, material is handled by the way of freeze-drying, is more beneficial for keeping volatile oil
Color and luster, fragrance, taste.
4th, present invention gained volatile oil yield is high (about 3%), and quality better, rich in unrighted acid, volatile oil carries
Taking technique no solvent residue, it is simple to operate, time-consuming it is short, be easy to industrialization.
5th, fermentation process is carried out using aspergillus, effectively reduces starch and fiber in malabar nut to extracting the shadow of active principle
Ring, improve the dissolution rate and yield of duckbilled flowers volatile oil.
6th, the resin in the technical process, solvent, eluant, eluent may be reused, and process costs are low, be easy to industrialize
Production.
Embodiment
With reference to specific embodiment, the invention will be further described, following examples be intended to illustrate invention rather than
Limitation of the invention further.
Embodiment 1
Dried malabar nut cauline leaf raw material is crushed to the mesh of 10 mesh~20,100Kg is weighed, enters extraction kettle after freeze-dried
SCF-CO 2 is carried out, duckbilled flowers volatile oil 1.54kg is obtained after about 2~4h.
Extraction residue is added into the rough spore aspergillus nutrient solutions of 10L, aerobic solid fermentation 3~5 days under the conditions of 28~30 DEG C.Hair
60~80% ethanol 800L, ultrasonic extraction 3 times under normal temperature, each 30min, three layers of filtered through gauze two are added after ferment in malabar nut
Secondary, ceramic membrane filter once, merging filtrate, is concentrated under reduced pressure at 50 DEG C and obtains dried object 6.2kg；By dried object 45L oil
Ether is extracted, and once, filtrate is concentrated under reduced pressure at 50 DEG C reclaims petroleum ether to ceramic membrane filter；Filter residue 3.72kg is obtained, adds 3L
PH=9 alkaline water dissolving, once, macroporous absorbent resin D101 carries out adsorbing separation to ceramic membrane filter on filtrate, and will collect
30% ethanol phase eluate be concentrated under reduced pressure drying, be concentrated under reduced pressure and obtain dried object 2.07kg, the ethanol content for adding 4L is
The 70% acidic ethanol aqueous solution is allowed to fully dissolve, 40 DEG C or so, adds 9L water；Ethanol containing adhatodine is molten
Liquid is placed on 4 DEG C of crystallizations overnight, obtains light yellow crystal, filters, obtain adhatodine crude product, be recrystallized to give adhatodine
1925g sterlings.Purity through HPLC detection adhatodine samples is 98.36%.
Comparative examples
Dried malabar nut cauline leaf raw material is crushed to the mesh of 10 mesh~20, is waved using extraction by steam distillation malabar nut
Hair oil, 100Kg is weighed, add water 1500L, put in volatile oil extractor and extracted, extract 4h.Distillate is extracted with hexamethylene,
Removed water with anhydrous sodium sulfate drying, low-temperature reduced-pressure recovery hexamethylene, obtain the pale yellow oily liquid of special odor, obtain duck
Mouth flowers volatile oil 0.19kg.
Residue after extraction adds 60~80% ethanol 800L, ultrasonic extraction 3 times under normal temperature, each 30min, three layers of yarn
Cloth filter twice, ceramic membrane filter once, merging filtrate, be concentrated under reduced pressure at 50 DEG C and obtain dried object 5.9kg；Dried object is used
50L petroleum ether is extracted, and once, filtrate is concentrated under reduced pressure at 50 DEG C reclaims petroleum ether to ceramic membrane filter；Obtain filter residue
3.43kg, 3.5L pH=9 alkaline water dissolving is added, once, macroporous absorbent resin D101 is inhaled ceramic membrane filter on filtrate
30% ethanol phase eluate of collection from and being concentrated under reduced pressure drying, be concentrated under reduced pressure and obtain dried object 1.89kg, add 4L by Fufen
Ethanol content be 70% the acidic ethanol aqueous solution be allowed to fully dissolve, 40 DEG C or so, add 9L water；Duckbilled will be contained
The ethanol solution of flower alkali is placed on 4 DEG C of crystallizations overnight, obtains light yellow crystal, filters, obtain adhatodine crude product, recrystallize
To adhatodine 1742g sterlings.Detected through HPLC, the purity of adhatodine sample is 98.21%.
Embodiment 2
Dried malabar nut cauline leaf raw material is crushed to the mesh of 10 mesh~20,200Kg is weighed, enters extraction kettle after freeze-dried
SCF-CO 2 is carried out, duckbilled flowers volatile oil 3.07kg is obtained after about 2~4h.
Residue after extraction adds the rough spore aspergillus nutrient solutions of 15L, aerobic solid fermentation 3~5 days under the conditions of 28~30 DEG C.
Malabar nut and 60~80% ethanol 1800L, ultrasonic extraction 3 times under normal temperature, each 30min, three layers of filtered through gauze two after fermentation
Secondary, ceramic membrane filter once, merging filtrate, is concentrated under reduced pressure at 50 DEG C and obtains dried object 11.4kg；By dried object 90L oil
Ether is extracted, and once, filtrate is concentrated under reduced pressure at 50 DEG C reclaims petroleum ether to ceramic membrane filter；Filter residue 7.4kg is obtained, adds 7L
PH=9 alkaline water dissolving, once, macroporous absorbent resin D101 carries out adsorbing separation to ceramic membrane filter on filtrate, and will collect
30% ethanol phase eluate be concentrated under reduced pressure drying, be concentrated under reduced pressure and obtain dried object 4.15kg, the ethanol content for adding 7L is
The 70% acidic ethanol aqueous solution is allowed to fully dissolve, 40 DEG C or so, adds 10L water；By the ethanol containing adhatodine
Solution is placed on 4 DEG C of crystallizations overnight, obtains light yellow crystal, filters, obtain adhatodine crude product, be recrystallized to give adhatodine
3821g sterlings.Detected through HPLC, the purity of adhatodine sample is 98.25%.
Embodiment 3
Dried malabar nut cauline leaf raw material is crushed to the mesh of 10 mesh~20,5Kg is weighed, enters after freeze-dried into extraction kettle
Duckbilled flowers volatile oil 772g is obtained after row SCF-CO 2, about 2~4h.
Residue after extraction adds the rough spore aspergillus nutrient solutions of 0.5L, the aerobic solid fermentation 3~5 under the conditions of 28~30 DEG C
My god.Malabar nut and 60~80% ethanol 40L, ultrasonic extraction 3 times under normal temperature, each 30min, three layers of filtered through gauze two after fermentation
Secondary, ceramic membrane filter once, merging filtrate, is concentrated under reduced pressure at 50 DEG C and obtains dried object 295g；By dried object 2.5L oil
Ether is extracted, and once, filtrate is concentrated under reduced pressure at 50 DEG C reclaims petroleum ether to ceramic membrane filter；Filter residue 187g is obtained, adds 0.2L
PH=9 alkaline water dissolving, once, macroporous absorbent resin D101 carries out adsorbing separation to ceramic membrane filter on filtrate, and will collect
30% ethanol phase eluate be concentrated under reduced pressure drying, be concentrated under reduced pressure and obtain dried object 102g, the ethanol content for adding 0.2L is
The 70% acidic ethanol aqueous solution is allowed to fully dissolve, 40 DEG C or so, adds 0.45L water；By the second containing adhatodine
Alcoholic solution is placed on 4 DEG C of crystallizations overnight, obtains light yellow crystal, filters, obtain adhatodine crude product, be recrystallized to give malabar nut
Alkali 95g sterlings.Detected through HPLC, the purity of adhatodine sample is 98.43%.
Claims (2)
1. producing the method for general flavone and volatile oil using malabar nut, its specific steps includes as follows：
(1) malabar nut cauline leaf is gathered annual 8~October, dried, crushed, cross 20 mesh sieves；
(2) the malabar nut stem and leaf powder to pulverize and sieve is added to supercritical CO2In the extraction kettle of extraction equipment, switch on power, connect
Logical refrigeration switch, controls the circulating water temperature in ice chest then to be begun to warm up in the range of 0~5 DEG C, and extracting pressure 15~
30MPa, 35~55 DEG C of extraction temperature, 2~4h of extraction time, two 30~40 DEG C of separating still temperature, separating still pressure 8~
152MPa, fill factor 80%, after extraction, gained liquid, as duckbilled flowers volatile oil are released from separating still；
(3) residue 5~10% rough spore aspergillus nutrient solutions of freeze-dried rear addition after extracting, the aerobic solid under the conditions of 28~30 DEG C
Fermentation 3~5 days；
(4) malabar nut after fermenting is at 20~40 DEG C, with the ethanol solution ultrasonic extraction 3 times of certain mass fraction, with ceramics
Membrane filtration, 3 times filtrate merges, and filtrate obtains the crude extract of general flavone, and dried at 50 DEG C through ethanol is recovered under reduced pressure；Will
Dried object is extracted with chloroform, and ceramic membrane filter obtains filter residue, and filtrate is concentrated under reduced pressure at 50 DEG C removes chloroform, vacuum drying；
(5) dried object is dissolved with a small amount of ethanol solution, pure with D101 types or AB-8 type macroreticular resins with ceramic membrane filter, filtrate
Change；Successively with deionized water, the ethanol elution of mass fraction 30%~90%, the as medicinal extract of collection ethanol phase, flavonoids
Compound crude extract.Recrystallized and dried with absolute ethyl alcohol after being concentrated under reduced pressure, it is dissolving crystallized with hot ethanol, add activated carbon to take off
Color, filtering, general flavone is obtained after freezing.
2. method according to claim 1, wherein the filter process is all to use ceramic membrane filter, fenestra pore size is
0.22μm。
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107987975A (en) * | 2017-12-21 | 2018-05-04 | 广东石油化工学院 | A kind of method of successive extract volatile oil and flavonoids in leaf from Exocarpium Citri Grandis |
| CN110693063A (en) * | 2019-11-13 | 2020-01-17 | 湖北中烟工业有限责任公司 | Preparation method of blueberry extract for cigarettes |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102888281A (en) * | 2012-10-19 | 2013-01-23 | 吉林人参研究院 | Method for extracting ginseng volatile oil by supercritical CO2 |
| CN104178350A (en) * | 2014-08-18 | 2014-12-03 | 安徽科技学院 | Method for separating and extracting chrysanthemum volatile oil, fiavonoid and phenolic acids from chrysanthemum |
| CN105497109A (en) * | 2016-01-12 | 2016-04-20 | 徐大鹏 | Process for producing milkvetch root total flavones through microbial fermentation technology |
-
2017
- 2017-08-09 CN CN201710673901.0A patent/CN107412292A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102888281A (en) * | 2012-10-19 | 2013-01-23 | 吉林人参研究院 | Method for extracting ginseng volatile oil by supercritical CO2 |
| CN104178350A (en) * | 2014-08-18 | 2014-12-03 | 安徽科技学院 | Method for separating and extracting chrysanthemum volatile oil, fiavonoid and phenolic acids from chrysanthemum |
| CN105497109A (en) * | 2016-01-12 | 2016-04-20 | 徐大鹏 | Process for producing milkvetch root total flavones through microbial fermentation technology |
Non-Patent Citations (3)
| Title |
|---|
| AWANTIKA SINGH ET: "Simultaneous determination of pyrroquinazoline alkaloids and flavonoids in Adhatoda beddomei and Adhatoda vasicaand their marketed herbal formulations using ultra high performance liquid chromatography coupled with triple quadrupole linear ion trap mass", 《BIOMEDICAL CHROMATOGRAPHY》 * |
| AWANTIKA SINGH: "Structural characterization of flavonoid C- and O -glycosides in an extract of Adhatoda vasica leaves by liquid chromatography with quadrupole time-of-flight mass spectrometry", 《RAPID COMMUN. MASS SPECTROM》 * |
| 郭力等: "《中药化学》", 31 August 2015, 中国医药科技出版社 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107987975A (en) * | 2017-12-21 | 2018-05-04 | 广东石油化工学院 | A kind of method of successive extract volatile oil and flavonoids in leaf from Exocarpium Citri Grandis |
| CN110693063A (en) * | 2019-11-13 | 2020-01-17 | 湖北中烟工业有限责任公司 | Preparation method of blueberry extract for cigarettes |
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