CN108434182A - A kind of supercritical CO2The method that fluid extraction technology extracts Leaves of Hippophae L polyphenol - Google Patents
A kind of supercritical CO2The method that fluid extraction technology extracts Leaves of Hippophae L polyphenol Download PDFInfo
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- CN108434182A CN108434182A CN201810312022.XA CN201810312022A CN108434182A CN 108434182 A CN108434182 A CN 108434182A CN 201810312022 A CN201810312022 A CN 201810312022A CN 108434182 A CN108434182 A CN 108434182A
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- 241000229143 Hippophae Species 0.000 title claims abstract description 47
- 150000008442 polyphenolic compounds Chemical class 0.000 title claims abstract description 40
- 235000013824 polyphenols Nutrition 0.000 title claims abstract description 40
- 239000000284 extract Substances 0.000 title claims abstract description 34
- 238000000605 extraction Methods 0.000 title claims description 74
- 235000003935 Hippophae Nutrition 0.000 title claims description 39
- 238000000034 method Methods 0.000 title claims description 19
- 239000012530 fluid Substances 0.000 title claims description 17
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 68
- 235000003145 Hippophae rhamnoides Nutrition 0.000 claims abstract description 9
- 238000002360 preparation method Methods 0.000 claims abstract description 6
- 229910002092 carbon dioxide Inorganic materials 0.000 claims description 24
- 239000000843 powder Substances 0.000 claims description 12
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 claims description 10
- 239000000463 material Substances 0.000 claims description 9
- 239000012141 concentrate Substances 0.000 claims description 8
- IDGUHHHQCWSQLU-UHFFFAOYSA-N ethanol;hydrate Chemical compound O.CCO IDGUHHHQCWSQLU-UHFFFAOYSA-N 0.000 claims description 8
- 239000001569 carbon dioxide Substances 0.000 claims description 5
- 238000010438 heat treatment Methods 0.000 claims description 4
- 238000007654 immersion Methods 0.000 claims description 4
- 238000004108 freeze drying Methods 0.000 claims description 3
- 238000005187 foaming Methods 0.000 claims 1
- 238000009777 vacuum freeze-drying Methods 0.000 claims 1
- 239000002253 acid Substances 0.000 abstract description 4
- 239000003963 antioxidant agent Substances 0.000 abstract description 4
- 230000003078 antioxidant effect Effects 0.000 abstract description 4
- HHEAADYXPMHMCT-UHFFFAOYSA-N dpph Chemical compound [O-][N+](=O)C1=CC([N+](=O)[O-])=CC([N+]([O-])=O)=C1[N]N(C=1C=CC=CC=1)C1=CC=CC=C1 HHEAADYXPMHMCT-UHFFFAOYSA-N 0.000 abstract description 4
- 230000007760 free radical scavenging Effects 0.000 abstract description 3
- 239000002994 raw material Substances 0.000 abstract description 2
- 235000019441 ethanol Nutrition 0.000 description 21
- 230000000694 effects Effects 0.000 description 7
- 239000000047 product Substances 0.000 description 4
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 3
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 description 3
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 241000196324 Embryophyta Species 0.000 description 2
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 description 2
- 239000004480 active ingredient Substances 0.000 description 2
- 238000004090 dissolution Methods 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 238000005057 refrigeration Methods 0.000 description 2
- 238000002390 rotary evaporation Methods 0.000 description 2
- 230000003068 static effect Effects 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- 235000001674 Agaricus brunnescens Nutrition 0.000 description 1
- 239000002028 Biomass Substances 0.000 description 1
- 241001117772 Elaeagnaceae Species 0.000 description 1
- 240000000950 Hippophae rhamnoides Species 0.000 description 1
- 208000031226 Hyperlipidaemia Diseases 0.000 description 1
- 206010028980 Neoplasm Diseases 0.000 description 1
- 244000197580 Poria cocos Species 0.000 description 1
- 235000008599 Poria cocos Nutrition 0.000 description 1
- 230000001476 alcoholic effect Effects 0.000 description 1
- 201000011510 cancer Diseases 0.000 description 1
- 230000032677 cell aging Effects 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 230000000295 complement effect Effects 0.000 description 1
- 230000006378 damage Effects 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 238000007598 dipping method Methods 0.000 description 1
- 238000002592 echocardiography Methods 0.000 description 1
- 235000013399 edible fruits Nutrition 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- 150000004676 glycans Chemical class 0.000 description 1
- 201000001421 hyperglycemia Diseases 0.000 description 1
- -1 mushroom Chemical class 0.000 description 1
- 239000012074 organic phase Substances 0.000 description 1
- 239000012071 phase Substances 0.000 description 1
- 229920001282 polysaccharide Polymers 0.000 description 1
- 239000005017 polysaccharide Substances 0.000 description 1
- 230000002265 prevention Effects 0.000 description 1
- 230000002250 progressing effect Effects 0.000 description 1
- 230000002000 scavenging effect Effects 0.000 description 1
- 239000002689 soil Substances 0.000 description 1
- 238000000194 supercritical-fluid extraction Methods 0.000 description 1
- 230000001360 synchronised effect Effects 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
- 238000003809 water extraction Methods 0.000 description 1
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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)
- A61K36/185—Magnoliopsida (dicotyledons)
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61P—SPECIFIC THERAPEUTIC ACTIVITY OF CHEMICAL COMPOUNDS OR MEDICINAL PREPARATIONS
- A61P3/00—Drugs for disorders of the metabolism
- A61P3/06—Antihyperlipidemics
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- A61P3/08—Drugs for disorders of the metabolism for glucose homeostasis
- A61P3/10—Drugs for disorders of the metabolism for glucose homeostasis for hyperglycaemia, e.g. antidiabetics
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61P—SPECIFIC THERAPEUTIC ACTIVITY OF CHEMICAL COMPOUNDS OR MEDICINAL PREPARATIONS
- A61P35/00—Antineoplastic agents
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- A61P—SPECIFIC THERAPEUTIC ACTIVITY OF CHEMICAL COMPOUNDS OR MEDICINAL PREPARATIONS
- A61P39/00—General protective or antinoxious agents
- A61P39/06—Free radical scavengers or antioxidants
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- 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
- A61K2236/33—Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones
- A61K2236/333—Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones using mixed solvents, e.g. 70% EtOH
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- 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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- 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
- A61K2236/50—Methods involving additional extraction steps
- A61K2236/51—Concentration or drying of the extract, e.g. Lyophilisation, freeze-drying or spray-drying
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Abstract
The invention discloses a kind of preparation methods of sea-buckthorn polyphenol extract, specifically use the sea-buckthorn leaf raw material after acid ethanol solution impregnates, pass through CO2The mode of supercritical extract carries out, and can get has total antioxidant capacity and DPPH free radical scavenging activities IC compared with prior art50Higher polyphenol extract.
Description
Technical field
The present invention relates to chemical composition extracting methods, particularly, are related to a kind of Leaves of Hippophae L polyphenol extracting method, especially relate to
And a kind of supercritical CO2The method of fluid extraction Leaves of Hippophae L polyphenol.
Background technology
Sea-buckthorn (Hippophaerhamnoides L.) is the shrub or small that Elaeangnaceae (Elaeagnaceae) acid thorn belongs to
Arbor.Sea-buckthorn is extensive in China's plantation, contains more than 200 kinds of nutriment in its root, stem, leaf, flower, fruit, has become China
A kind of excellent economic tree to conserve water and soil that three northern areas of China are largely being developed.Leaves of Hippophae L as waste contains abundant
Polyphenols is the main active ingredient of Leaves of Hippophae L, is had in prevention hyperglycemia, hyperlipidemia, cancer, cell ageing etc.
Fine effect.
Previous researcher extracts Leaves of Hippophae L polyphenol and uses water extraction, microwave method, supercritical ultrasonics technology etc., these traditional extraction sides
Method often operating cost when, may result in Leaves of Hippophae L polyphenol extract activity reduce etc. undesirable result.
Supercritical fluid extraction is the special nature possessed by Near The Critical Point and the emerging extraction that is formed using fluid
Technology.Supercritical CO2It is a kind of most-often used fluid, it is neither liquid, nor gas, but have the high density of liquid
With the property of the low viscosity of gas, therefore there are higher solvability and higher diffusion, can adequately be mixed with sample
It closes, contact, plays its solvability to greatest extent.In order to improve the selectivity to some polar substances, face frequently with super
Boundary CO2The method that suitable entrainer (or modifying agent) is added in extraction system, common entrainer have methanol, ethyl alcohol, acetone,
Ethyl acetate, water etc. improve CO using entrainer2Fluid dissolution properties so that supercritical CO2Extract the strong object of polyphenol isopolarity
Matter is possibly realized.
Although utilizing supercritical CO2Fluid extraction technology has extracted the research of certain plants polysaccharide (such as mushroom, Poria cocos)
It has been reported that, but uses supercritical CO2The research of fluid extraction technology extraction Leaves of Hippophae L polyphenol has not been reported.
For this purpose, this research is to prepare high activity Leaves of Hippophae L polyphenol as target, using the supercritical CO of addition entrainer2Extraction
Mode extracts Leaves of Hippophae L polyphenol, rationally to be provided using the abundant Leaves of Hippophae L resource of biomass and preparation high activity Leaves of Hippophae L polyphenol
Guidance.
Invention content
The purpose of the present invention is intended to china natural resources very abundant and the Leaves of Hippophae L that effective exploitation utilizes is not yet received as plant
Object material provides a kind of efficient supercritical CO2The preparation method of fluid extraction Leaves of Hippophae L polyphenol.
1, a kind of through supercritical CO2The method of fluid preparation Leaves of Hippophae L polyphenol extract comprising step：
(1) the Leaves of Hippophae L powder for being crushed to 20 mesh being mixed with ethanol solution, soaked overnight (10-24h) obtains immersion material,
Material will be impregnated to fill in 300 milliliters of extraction kettles, the quality of the Leaves of Hippophae L powder is 1 with the volume ratio of the ethanol solution:
1, the ethanol solution is the ethanol water that volume fraction is 60%, and the volume unit of the ethanol solution is milliliter, described
Leaves of Hippophae L powder sample quality unit is gram；60% ethanol water pH is 3-4.
(2) extraction kettle filled is fixed in heater box, all air valves should all close shape in system at this time
State connects two end interface of extraction kettle, shuts heating chamber door, wherein all air valves include air inlet switch, air outlet valve and
Reset valve；
(3) supercritical CO is opened2Fluid extraction apparatus power supply, setting extraction kettle temperature, reset valve temperature, waits for that temperature reaches
When setting value, opens air inlet switch and adjust extraction kettle pressure, kept after extraction kettle pressure reaches setting condition, under the conditions of this
5min, wherein the extraction kettle temperature is 40 DEG C, the reset valve temperature is 90 DEG C, and the extraction kettle pressure is
30MPa；
(4) air outlet valve is opened, utilizes gas flow in reset valve control returnable bottle so that the flowmeter that tail connects shows flow
For 2L/min, balance extraction kettle pressure is pumped by carbon dioxide pneumatic, keeps extraction kettle pressure constant, opens entrainer pump, control
Entrainer flow velocity processed after extraction time reaches, closes air inlet switch, allows CO in extraction kettle2Continue to be discharged, returnable bottle continues to collect
Extract, until CO2Emptying, removes returnable bottle, wherein the entrainer is the ethanol solution of 60% volume fraction, entrainer
Flow velocity is 1.5ml/min, and the extraction time is 1.5 hours；
(5) extracting solution in the returnable bottle is gone in concentrate bottle, is concentrated on a rotary evaporator, rotary evaporation
Instrument vacuum degree 0.09Mpa, bath temperature control is poured at 50 DEG C, then by the solution in concentrate bottle in surface plate, in vacuum refrigeration
Freeze-drying, obtains Leaves of Hippophae L polyphenol extract in drying machine.
There are three the difference of technical solution of the present invention and the prior art is main：
1, Leaves of Hippophae L powder is stayed overnight with alcohol solution dipping；
2, the ethanol water that the solution is 60%, pH 3-4；
3, static extracting and dynamic extraction substep carry out in extraction process, rather than conventional synchronous progress.
Three above difference has technical effect that：
1, due to CO2For apolar substance, Leaves of Hippophae L polyphenol is in supercritical CO2Solubility in fluid is relatively low, directly extracts
Yield is relatively low, and first uses the Leaves of Hippophae L powder of ethyl alcohol soaked overnight, can both make the dissolving of sub-fraction polyphenol in ethanol, simultaneously
Also other polyphenol components are promoted to be in a kind of state to be dissolved out being activated, to contribute to CO2Extraction when supercritical extract
It takes；
2, inventor has found simultaneously, by the adjustment of the pH value of ethanol water slant acidity range, contribute to Polyphenols at
The dissolution of split-phase organic phase, this also helps to what entrainer when the effect and supercritical extract of ethyl alcohol soaked overnight acted on
It plays so that CO2The efficiency of supercritical extract obtains whole promotion；
3, when supercritical extract, the process of static extracting is first taken, using certain temperature and pressure, is promoted and extracts early period
Efficiency and active ingredient extraction, the later stage uses the process of dynamic extraction, realizes the further extraction of polyphenol components, two
Process organically combines, and promotes extraction efficiency as much as possible.
Inventor is pointed out that above-described three inventive points are complementary three key steps, front and back
It echoes, realizes effective extraction of sea-buckthorn polyphenol components together, meanwhile, for the parameter setting in each step, inventor
Selection is optimized.
The Leaves of Hippophae L polyphenol extract that the present invention obtains is characterized in：Product material object yield 3.7% or so, wherein sea-buckthorn is more
Phenol accounts for 5.9% of extract or so, and the total antioxidant capacity (being indicated with Vc equivalents) of polyphenol extract is extracted for 8.44mgVc/g
Object, DPPH free radical scavenging activities IC50For 10.05 μ g/mL；At the same time, using sea-buckthorn made from conventional ultrasonic wave extractive technique
Leaf polyphenol extract total antioxidant capacity is 6.15mg Vc/g extracts, DPPH free radical scavenging activities IC50For 20.19 μ g/mL,
Compare the activity for the Leaves of Hippophae L polyphenol extract that two kinds of techniques obtain, Leaves of Hippophae L is more made from supercritical carbon dioxide extractive technique
Total antioxidant ability of phenol is 1.37 times of ultrasonic wave extraction prepared product, and DPPH Scavenging activities are ultrasonic wave extraction prepared products
2.01 again.
It it not is 1.66 times using soak extraction yield using the extraction yield impregnated.
Ethanol solution acid adding tune pH, yield are do not adjust pH 2.10 times.
A specific scheme can be：
It is a kind of through supercritical CO2The method of fluid preparation Leaves of Hippophae L polyphenol, step are：
(1) the Leaves of Hippophae L powder for being crushed to 20 mesh is mixed with ethanol solution, soaked overnight obtains immersion material, by soak
Material is filled in 300 milliliters of extraction kettles, and the quality of the Leaves of Hippophae L powder is 1 with the volume ratio of the ethanol solution:1, the second
Alcoholic solution is the ethanol water that volume fraction is 60%, and the volume unit of the ethanol solution is milliliter, the Leaves of Hippophae L powder
Sample quality unit is gram；
(2) extraction kettle filled is fixed in heater box, all air valves should all close shape in system at this time
State connects two end interface of extraction kettle, shuts heating chamber door, wherein all air valves include air inlet switch, air outlet valve and
Reset valve；
(3) supercritical CO is opened2Fluid extraction apparatus power supply, setting extraction kettle temperature, reset valve temperature, waits for that temperature reaches
When setting value, opens air inlet switch and adjust extraction kettle pressure, kept after extraction kettle pressure reaches setting condition, under the conditions of this
5min, wherein the extraction kettle temperature is 40 DEG C, the reset valve temperature is 90 DEG C, and the extraction kettle pressure is
30MPa；
(4) air outlet valve is opened, utilizes gas flow in reset valve control returnable bottle so that the flowmeter that tail connects shows flow
For 2L/min, balance extraction kettle pressure is pumped by carbon dioxide pneumatic, keeps extraction kettle pressure constant, opens entrainer pump, control
Entrainer flow velocity processed after extraction time reaches, closes air inlet switch, allows CO in extraction kettle2Continue to be discharged, returnable bottle continues to collect
Extract, until CO2Emptying, removes returnable bottle, wherein the entrainer is the ethanol solution of 60% volume fraction, entrainer
Flow velocity is 1.5ml/min, and the extraction time is 1.5 hours；
(5) extracting solution in the returnable bottle is gone in concentrate bottle, is concentrated on a rotary evaporator, rotary evaporation
Instrument vacuum degree 0.09Mpa, bath temperature control is poured at 50 DEG C, then by the solution in concentrate bottle in surface plate, in vacuum refrigeration
Freeze-drying, obtains Leaves of Hippophae L polyphenol extract in drying machine.
Specific implementation mode
Embodiment 1. prepares Leaves of Hippophae L polyphenol extract
The Leaves of Hippophae L powder 100g of 20 mesh is mixed with 60% ethanol solutions of 100ml (pH 4), soaked overnight, by soak
The extraction kettle filled is fixed in heater box loaded in 300 milliliters of extraction kettles, connects two end interface of extraction kettle by material, closes
Air inlet switch, air outlet valve and reset valve are closed, heating chamber door is shut；Open supercritical CO2Fluid extraction apparatus power supply, setting extraction
90 DEG C of 40 DEG C of kettle temperature degree and reset valve temperature open air inlet switch when temperature reaches setting value, adjust extraction kettle pressure and are
30MPa keeps 10min under this pressure condition；Air outlet valve is opened, gas flow in reset valve control returnable bottle is utilized so that
The flowmeter that tail connects shows that flow is 2L/min, pumps balance extraction kettle pressure by carbon dioxide pneumatic, keeps extraction kettle pressure
It is constant, entrainer pump is opened, the ethanol solution flow velocity of 60% volume fraction of control is 1.5ml/min, extracts 1.5 hours, closes
Air inlet switch, allows CO in extraction kettle2Continue to be discharged, returnable bottle continues to collect extract, until CO2Emptying, removes returnable bottle；It will
Extracting solution in returnable bottle is gone in concentrate bottle, is concentrated on a rotary evaporator, rotavapor under vacuum degree 0.09Mpa,
Bath temperature control is poured at 50 DEG C, then by the solution in concentrate bottle in surface plate, in being lyophilized in vacuum freeze drier, is obtained dry
Leaves of Hippophae L polyphenol extract 3.7g after dry, wherein polyphenol account for the 5.9% of extract.
Embodiment 2
The influence that ethyl alcohol impregnates
Contrast test is carried out with unsoaked mode using impregnating, it is each to carry out carrying out yield and polyphenol content comparison three times,
The results obtained are as follows：
| (yield/polyphenol content) | 1 | 2 | 3 | It is average |
| It impregnates | 3.69/5.91 | 3.71/5.88 | 3.69/5.90 | 3.70/5.90 |
| It does not impregnate | 2.22/4.55 | 2.24/4.55 | 2.23/4.51 | 2.23/4.54 |
As can be seen from the above table, whether from final product yield or the polyphenol content extracted, using elder generation
The mode extracted after immersion has significant progress.
Embodiment 3
The influence of ethanol solution pH
The mode that inventor uses gradient type carries out contrast test, with ethyl alcohol original solution (ph is probably 6.9 or so),
6.5,6.0,5.5,5.0,4.5,4.0,3.5,3.0,2.5,2.0,1.5 pH value carries out, and the results obtained are as follows：
From experimental result as can be seen that originally when ethanol solution pH gradient reduces, yield and polyphenol content have larger amplitude
Stable state is presented when pH is between 3-4 substantially for the promotion of degree, and work as pH reduces again, when progressing into strong acid area, yield
The state of rapid decrease is showed with polyphenol content, inventor speculates that too strong acidity is possible to repercussion and results in raw material mix
Deng destruction, it is final to influence product yield etc..
Claims (3)
1. a kind of through supercritical CO2The method of fluid preparation Leaves of Hippophae L polyphenol extract comprising step：
(1) the Leaves of Hippophae L powder for being crushed to 20 mesh is mixed with ethanol solution, soaked overnight (10-24h) obtains immersion material, will soak
Foaming material is filled in 300 milliliters of extraction kettles, and the quality of the Leaves of Hippophae L powder is 1 with the volume ratio of the ethanol solution:1, institute
It is the ethanol water that volume fraction is 60% to state ethanol solution, and the volume unit of the ethanol solution is milliliter, the sea-buckthorn
Leaf powder sample quality unit is gram；60% ethanol water is acidity.
(2) extraction kettle filled is fixed in heater box, all air valves all should in off position, even in system at this time
Two end interface of extraction kettle is connected, heating chamber door is shut, wherein all air valves include air inlet switch, air outlet valve and fine tuning
Valve；
(3) supercritical CO is opened2Fluid extraction apparatus power supply, setting extraction kettle temperature, reset valve temperature, waits for that temperature reaches setting
When value, opens air inlet switch and adjusts extraction kettle pressure, 5min is kept after extraction kettle pressure reaches setting condition, under the conditions of this,
Wherein the extraction kettle temperature is 40 DEG C, and the reset valve temperature is 90 DEG C, and the extraction kettle pressure is 30MPa；
(4) air outlet valve is opened, utilizes gas flow in reset valve control returnable bottle so that the flowmeter that tail connects shows that flow is
2L/min pumps balance extraction kettle pressure by carbon dioxide pneumatic, keeps extraction kettle pressure constant, opens entrainer pump, control
Entrainer flow velocity after extraction time reaches, closes air inlet switch, allows CO in extraction kettle2Continue to be discharged, returnable bottle, which continues to collect, to be carried
Object is taken, until CO2Emptying, removes returnable bottle, wherein the entrainer is the ethanol solution of 60% volume fraction, entrainer stream
Speed is 1.5ml/min, and the extraction time is 1.5 hours；
(5) extracting solution in the returnable bottle is gone in concentrate bottle, is concentrated on a rotary evaporator, Rotary Evaporators are true
Reciprocal of duty cycle 0.09Mpa, bath temperature control is poured at 50 DEG C, then by the solution in concentrate bottle in surface plate, in vacuum freeze drying
Freeze-drying, obtains Leaves of Hippophae L polyphenol extract in machine.
2. according to the method for claim, wherein the pH of described 60% ethanol water is 3-4.
3. Leaves of Hippophae L polyphenol extract made from the method according to claims 1 or 2.
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| CN201810312022.XA CN108434182B (en) | 2018-04-09 | 2018-04-09 | Supercritical CO2Method for extracting seabuckthorn leaf polyphenol by fluid extraction technology |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109865419A (en) * | 2019-02-28 | 2019-06-11 | 河南传宇生物科技有限公司 | A kind of plant eliminating smell agent and preparation method thereof |
| CN113797182A (en) * | 2021-10-14 | 2021-12-17 | 云南博瑞生物科技有限公司 | Method for preparing lutein oil suspension |
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| CN113797182A (en) * | 2021-10-14 | 2021-12-17 | 云南博瑞生物科技有限公司 | Method for preparing lutein oil suspension |
| CN113797182B (en) * | 2021-10-14 | 2023-03-10 | 云南博瑞生物科技有限公司 | Method for preparing lutein oil suspension |
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