CN105861144A - Supercritical extraction technology of cynomorium songaricum oil - Google Patents
Supercritical extraction technology of cynomorium songaricum oil Download PDFInfo
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- CN105861144A CN105861144A CN201610371077.9A CN201610371077A CN105861144A CN 105861144 A CN105861144 A CN 105861144A CN 201610371077 A CN201610371077 A CN 201610371077A CN 105861144 A CN105861144 A CN 105861144A
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- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
- C11B1/00—Production of fats or fatty oils from raw materials
- C11B1/02—Pretreatment
- C11B1/04—Pretreatment of vegetable raw material
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- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
- C11B1/00—Production of fats or fatty oils from raw materials
- C11B1/10—Production of fats or fatty oils from raw materials by extracting
- C11B1/104—Production of fats or fatty oils from raw materials by extracting using super critical gases or vapours
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
- C11B3/00—Refining fats or fatty oils
- C11B3/16—Refining fats or fatty oils by mechanical means
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- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Oil, Petroleum & Natural Gas (AREA)
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- Organic Chemistry (AREA)
- Mechanical Engineering (AREA)
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- Extraction Or Liquid Replacement (AREA)
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Abstract
The invention relates to a supercritical extraction technology of cynomorium songaricum oil. The technology comprises the following steps: grinding: grinding the stem of cynomorium songaricum to obtain cynomorium songaricum powder; drying: drying the cynomorium songaricum powder and sieving; extraction: extracting the sieved cynomorium songaricum powder by using a supercritical CO2 fluid to obtain a cynomorium songaricum oil extract; and centrifugal separation: performing centrifugal separation on the cynomorium songaricum oil extract to obtain the cynomorium songaricum oil. The supercritical extraction technology of the cynomorium songaricum oil, provided by the invention, has the advantages of high extraction rate, low extraction cost, no solvent residue, short extraction period and no environmental pollution and can provide a technical support for small-batch production of special oil.
Description
Technical field
The present invention relates to biochemical field, in particular it relates to the supercritical extraction process of a kind of Herba Cynomorii oil.
Background technology
Vegetable oil lipoprotein is one of mankind's important sources obtaining essential fatty acid, and the chemical industry being also important is former
Material.Along with people's further investigation to vegetable oil resource, many physiological functions of Vegetable oil lipoprotein and effect by
Gradually it is found.Meanwhile, people increasingly pay attention to the research of the extracting process of the oils and fats of different purposes, to obtaining
Obtain Vegetable oil lipoprotein extraction scheme the most economic, that be suitable for.
Acquisition methods predominantly organic tool milling process, solvent extraction method and the water substitution of existing Vegetable oil lipoprotein.Wherein, machine
It is low to there is oil yield in tool milling process, and labor intensity is big, produces the shortcoming that effect is low, and due to oil expression during
Having green compact to steam the operation fried, protein denaturation is serious, and oil resource is made a low multiple use.Solvent extraction method extracts out
The crude oil come is more containing non-oil substances, and color and luster is relatively deep, second-rate, and it is inflammable and explosive to leach solvent for use,
And there is certain toxicity, the poor stability of production and the residual of solvent in oils and fats can be caused.Water substitution carries oil
Major defect be that oil yield is less than tradition solvent extraction method, easy contaminating microorganisms in leaching process, and discharging
Substantial amounts of waste water need to process.
The oil resource that the plant resources being grown in desert is extracted, because of its residing growing environment, often has
There is higher antioxidant activity.Therefore, extract and develop psammophytes oil resource and have broad prospects.
Herba Cynomorii resource is one of important psammophytes resource, but its oil content is low, there is traditional method and is difficult to extract,
Traditional extraction process is not yet had to be applied to the case that Herba Cynomorii oil extracts at present.Meanwhile, big because Herba Cynomorii oil contains
The oxygen-containing fatty acid of antioxidation of amount, the high temperature parch of other technique necessarily destroys its structure, thus is allowed to lose
Antioxidant activity.
Summary of the invention
The present inventor is found by research, and supercritical extraction can be close to room temperature (35 DEG C~40 DEG C)
And fluid shroud under extract, effectively prevent oxidation and the loss of heat-sensitive substance.Therefore, exist
Extract remains the effective ingredient of medicinal plants, and can be high boiling point, low volatility, easily pyrolysis
Material extracts under far below its boiling temperature.
Wherein, supercritical CO2Abstraction technique has good solvent property because of it, is widely used in and plants
The extraction of thing oils and fats.Additionally, supercritical CO2Abstraction technique has the further advantage that 1) because of CO2It is one
Plant inactive gas, extraction process does not occur chemical reaction, and belongs to non-flammable gases, tasteless, nothing
It is smelly, nontoxic, so safety is the best;2) owing to overall process is without organic solvent, therefore extract is absolutely not
The vehicle substance of residual, thus prevent the existence of harmful thing in extraction process and the pollution to environment;
3) selectivity is good.CO2Solvability can be controlled, thus selectively by regulation temperature and pressure
Extraction purpose product, reduces impurity and makes the effective ingredient of purpose product highly enriched, improve product quality and
Outward appearance, and technique is simple, time saving and energy saving;4)CO2Gas price is cheap, and purity is high, easily produces, and
Can use with repetitive cycling aborning, thus cost can be effectively reduced.
It is contemplated that one of technical problem solved the most to a certain extent in correlation technique.
To this end, it is an object of the present invention to propose a kind of low cost, extraction yield height, no solvent residue,
The supercritical extraction process that cycle Herba Cynomorii short, non-environmental-pollution is oily.
The supercritical extraction process of a kind of Herba Cynomorii oil according to embodiments of the present invention, comprises the steps: to pulverize:
The stem of Herba Cynomorii is pulverized, to obtain Songaria Cynomorium Herb;Dry: Songaria Cynomorium Herb is dried, sieves;Extraction: profit
Use supercritical CO2Songaria Cynomorium Herb after sieving is extracted by fluid, to obtain Herba Cynomorii oil extract;Centrifugal
Separate: by Herba Cynomorii oil extract centrifugation, to obtain Herba Cynomorii oil.
The supercritical extraction process of a kind of Herba Cynomorii oil according to embodiments of the present invention, extraction yield reaches more than 2%,
It is obviously improved the extraction yield of Herba Cynomorii oil.Meanwhile, the supercritical CO that the present invention uses2Extracting process, with super
CO under critical state2Fluid, as extractant, has extraction low cost, no solvent residue, extraction cycle
The features such as short, non-environmental-pollution, it is possible to the production for small lot special oil provides technical support.
It addition, the supercritical extraction process of a kind of Herba Cynomorii according to the above embodiment of the present invention oil, it is also possible to tool
There is a following additional technical characteristic:
Further, in extraction step, supercritical CO2The extracting pressure of fluid is 20MPa~30MPa,
Extraction temperature 35 DEG C~45 DEG C, CO2Fluid flow is 12mL/min~20mL/min, and extraction time is
1.5h~2.5h.
Further, in extraction step, supercritical CO2The extracting pressure of fluid is 30MPa, extraction temperature
Spend 40 DEG C, CO2Fluid flow is 12mL/min, and extraction time is 2.5h.
Further, in extraction step, supercritical CO2The extracting pressure of fluid is 30MPa, extraction temperature
Spend 45 DEG C, CO2Fluid flow is 12mL/min, and extraction time is 2.5h.
Further, in extraction step, supercritical CO2The extracting pressure of fluid is 20MPa, extraction temperature
Spend 35 DEG C, CO2Fluid flow is 15mL/min, and extraction time is 1.5h.
Further, in extraction step, supercritical CO2The extracting pressure of fluid is 25MPa, extraction temperature
Spend 38 DEG C, CO2Fluid flow is 18mL/min, and extraction time is 1.8h.
Further, in extraction step, supercritical CO2The extracting pressure of fluid is 28MPa, extraction temperature
Spend 42 DEG C, CO2Fluid flow is 20mL/min, and extraction time is 2.2h.Further, step is being dried
In Zhou, drying temperature is 30 DEG C~40 DEG C, and drying time is 18h~30h.
Further, in pulverising step, the aperture of screen cloth is 0.177 μm~0.25 μm.
Further, in step with centrifugal separation, rotating speed is 10000r/min~12000r/min, centrifugation
Time be 10min~30min.
The additional aspect of the present invention and advantage will part be given in the following description, and part will be retouched from following
Become obvious in stating, or recognized by the practice of the present invention.
Detailed description of the invention
Below in conjunction with detailed description of the invention, the present invention is further detailed explanation.
Embodiment 1
The supercritical CO of Herba Cynomorii oil2The key step of extraction is as follows:
The first step, goes the Herba Cynomorii stem removing inflorescence gathered to the removal of impurity, pulverizes, to obtain Songaria Cynomorium Herb.
Second step, is placed in Songaria Cynomorium Herb at 30 DEG C~40 DEG C drying, is 0.177 μm~0.25 μm with aperture
Screen cloth sieves.
3rd step, utilizes supercritical CO2Songaria Cynomorium Herb after sieving is extracted by fluid, fluid extraction pressure
Power is 20~30MPa, extraction temperature 35 DEG C~45 DEG C, CO2Fluid flow is 12ml/min~20ml/min,
L.5h~2.5h extraction time is, obtains Herba Cynomorii oil extract.
4th step, in the environment of room temperature 20 DEG C~30 DEG C, Herba Cynomorii oil extract is positioned over rotating speed is
In the high speed centrifuge of 10000r/min~12000r/min, centrifugal 10min~30min, removes impurity, obtains
Herba Cynomorii oil.
Wherein, second step, Songaria Cynomorium Herb is placed at 30 DEG C drying 24h, with the sieve that aperture is 0.177 μm
Net sieves.3rd step, each factor range extracted according to general oils and fats arranges the orthogonal reality of 4 factor 3 levels
Test design, totally 9 groups of tests.4th step, is positioned over Herba Cynomorii oil extract in the environment of room temperature 25 DEG C and turns
Speed be 12000r/min high speed centrifuge in centrifugal 10 minutes, remove impurity, obtain Herba Cynomorii oil.
Table 1 orthogonal design factor and water-glass
Orthogonal Experiment and Design acquired results shows, in designed factor and level with fluid extraction pressure is
30MPa, extraction temperature is 40 DEG C, CO2Fluid flow 12ml/min, extraction effect when extraction time is 2.5h
Preferably, extraction ratio is 2.57% to fruit.Through orthogonal experiment software analysis, the optimum extraction conditions after orthogonal optimization
For fluid extraction pressure 30MPa, extraction temperature 45 DEG C, CO2Fluid flow 12ml/min, extraction time
2.5h。
Embodiment 2
The supercritical CO of Herba Cynomorii oil2The key step of extraction is as follows:
The first step, goes the Herba Cynomorii stem removing inflorescence gathered to the removal of impurity, pulverizes, to obtain Songaria Cynomorium Herb.
Second step, is placed in Songaria Cynomorium Herb at 30 DEG C drying 24h, sieves with the screen cloth that aperture is 0.177 μm.
3rd step, utilizes supercritical CO2Songaria Cynomorium Herb after sieving is extracted by fluid, fluid extraction pressure
Power is 30MPa, extraction temperature 40 DEG C, CO2Fluid flow is 12ml/min, and extraction time is 2.5h,
To Herba Cynomorii oil extract.
4th step, is at room temperature positioned over, by Herba Cynomorii oil extract, the high speed centrifuge that rotating speed is 12000r/min
In centrifugal 10 minutes, remove impurity, obtain Herba Cynomorii oil.Herba Cynomorii oil extraction rate reached is to 2.78%.
Embodiment 3
The first step, goes the Herba Cynomorii stem removing inflorescence gathered to the removal of impurity, pulverizes, to obtain Songaria Cynomorium Herb.
Second step, is placed in Songaria Cynomorium Herb at 40 DEG C drying, sieves with the screen cloth that aperture is 0.25 μm.
3rd step, utilizes supercritical CO2Songaria Cynomorium Herb after sieving is extracted by fluid, fluid extraction pressure
Power is 30MPa, extraction temperature 45 DEG C, CO2Fluid flow is 12ml/min, and extraction time is 2.5h,
To Herba Cynomorii oil extract.
4th step, it is 12000r/min's that Herba Cynomorii oil extract is positioned in the environment of room temperature 25 DEG C rotating speed
High speed centrifuge is centrifuged 10 minutes, removes impurity, obtain Herba Cynomorii oil.Herba Cynomorii oil extraction rate reached is to 2.64%.
Embodiment 4
The first step, goes the Herba Cynomorii stem removing inflorescence gathered to the removal of impurity, pulverizes, to obtain Songaria Cynomorium Herb.
Second step, is placed in Songaria Cynomorium Herb at 40 DEG C drying, sieves with the screen cloth that aperture is 0.25 μm.
3rd step, utilizes supercritical CO2Songaria Cynomorium Herb after sieving is extracted by fluid, fluid extraction pressure
Power is 20MPa, extraction temperature 35 DEG C, CO2Fluid flow is 15ml/min, and extraction time is 1.5h,
To Herba Cynomorii oil extract.
4th step, it is 12000r/min's that Herba Cynomorii oil extract is positioned in the environment of room temperature 25 DEG C rotating speed
High speed centrifuge is centrifuged 10 minutes, removes impurity, obtain Herba Cynomorii oil.Herba Cynomorii oil extraction rate reached is to 2.59%.
Embodiment 5
The first step, goes the Herba Cynomorii stem removing inflorescence gathered to the removal of impurity, pulverizes, to obtain Songaria Cynomorium Herb.
Second step, is placed in Songaria Cynomorium Herb at 40 DEG C drying, sieves with the screen cloth that aperture is 0.25 μm.
3rd step, utilizes supercritical CO2Songaria Cynomorium Herb after sieving is extracted by fluid, fluid extraction pressure
Power is 25MPa, extraction temperature 38 DEG C, CO2Fluid flow is 18ml/min, and extraction time is 1.8h,
To Herba Cynomorii oil extract.
4th step, it is 12000r/min's that Herba Cynomorii oil extract is positioned in the environment of room temperature 25 DEG C rotating speed
High speed centrifuge is centrifuged 10 minutes, removes impurity, obtain Herba Cynomorii oil.Herba Cynomorii oil extraction rate reached is to 2.46%.
Comparative example 1
The first step, goes the Herba Cynomorii stem removing inflorescence gathered to the removal of impurity, pulverizes, to obtain Songaria Cynomorium Herb.
Second step, is placed in Songaria Cynomorium Herb at 40 DEG C drying, sieves with the screen cloth that aperture is 0.25 μm.
3rd step, utilizes supercritical CO2Songaria Cynomorium Herb after sieving is extracted by fluid, fluid extraction pressure
Power is 16MPa, extraction temperature 48 DEG C, CO2Fluid flow 10ml/min, extracts 1h, obtains Herba Cynomorii oil
Extract.
4th step, it is 12000r/min's that Herba Cynomorii oil extract is positioned in the environment of room temperature 25 DEG C rotating speed
High speed centrifuge is centrifuged 10 minutes, removes impurity, obtain Herba Cynomorii oil.Herba Cynomorii oil extraction rate reached is to 0.82%.
Comparative example 2
The first step, goes the Herba Cynomorii stem removing inflorescence gathered to the removal of impurity, pulverizes, to obtain Songaria Cynomorium Herb.
Second step, is placed in Songaria Cynomorium Herb at 40 DEG C drying, sieves with the screen cloth that aperture is 0.25 μm.
3rd step, utilizes supercritical CO2Songaria Cynomorium Herb after sieving is extracted by fluid, fluid extraction pressure
Power is 23MPa, extraction temperature 20 DEG C, CO2Fluid flow 30ml/min, extracts 3h, obtains Herba Cynomorii oil
Extract.
4th step, it is 12000r/min's that Herba Cynomorii oil extract is positioned in the environment of room temperature 25 DEG C rotating speed
High speed centrifuge is centrifuged 10 minutes, removes impurity, obtain Herba Cynomorii oil.Herba Cynomorii oil extraction rate reached is to 1.09%.
Comparative example 3
The first step, goes the Herba Cynomorii stem removing inflorescence gathered to the removal of impurity, pulverizes, to obtain Songaria Cynomorium Herb.
Second step, is placed in Songaria Cynomorium Herb at 40 DEG C drying, sieves with the screen cloth that aperture is 0.25 μm.
3rd step, utilizes supercritical CO2Songaria Cynomorium Herb after sieving is extracted by fluid, fluid extraction pressure
Power is 18MPa, extraction temperature 50 DEG C, CO2Fluid flow 21ml/min, extracts 1.5h, obtains Herba Cynomorii oil
Extract.
4th step, it is 12000r/min's that Herba Cynomorii oil extract is positioned in the environment of room temperature 25 DEG C rotating speed
High speed centrifuge is centrifuged 10 minutes, removes impurity, obtain Herba Cynomorii oil.Herba Cynomorii oil extraction rate reached is to 0.97%.
The Herba Cynomorii oil extracting the embodiment of the present invention or comparative example uses GC-MS to carry out component analysis, result
Show with the unsaturated fatty acid containing high level in Herba Cynomorii oil, and unsaturated fatty acid is biological active matter
Matter, this shows that Herba Cynomorii oil has higher Development volue.
By comparing embodiment and comparative example it appeared that the most optimized CO2Supercritical extraction rate typically exists
About 1%, and extraction yield according to embodiments of the present invention reaches more than 2%, has been obviously improved the extraction of Herba Cynomorii oil
Take rate.Meanwhile, the supercritical CO that the present invention uses2Extraction process, with the CO under above-critical state2Fluid is made
For extractant, there is the features such as extraction low cost, no solvent residue, short, the non-environmental-pollution of extraction cycle,
Technical support can be provided for the production of small lot special oil.
By comparing embodiment and comparative example it appeared that the most optimized CO2Supercritical extraction rate typically all exists
About 1%, and extraction yield according to embodiments of the present invention reaches more than 2%, has been obviously improved the extraction of Herba Cynomorii oil
Take rate.Meanwhile, the supercritical CO that the present invention uses2Extraction process, with the CO under above-critical state2Fluid is made
For extractant, there is the features such as extraction low cost, no solvent residue, short, the non-environmental-pollution of extraction cycle,
Technical support can be provided for the production of small lot special oil.
In the description of this specification, reference term " embodiment ", " some embodiments ", " example ",
The description of " concrete example " or " some examples " etc. means to combine this embodiment or example describes specific features,
Structure, material or feature are contained at least one embodiment or the example of the present invention.In this manual,
The schematic representation of above-mentioned term is necessarily directed to identical embodiment or example.And, description
Specific features, structure, material or feature can with in one or more embodiments in office or example with suitably
Mode combines.Additionally, in the case of the most conflicting, those skilled in the art can be by this specification
Described in different embodiments or the feature of example and different embodiment or example be combined and combine.
Although above it has been shown and described that embodiments of the invention, it is to be understood that above-described embodiment
It is exemplary, it is impossible to being interpreted as limitation of the present invention, those of ordinary skill in the art is the present invention's
In the range of above-described embodiment can be changed, revise, replace and modification.
Claims (10)
1. the supercritical extraction process of a Herba Cynomorii oil, it is characterised in that comprise the steps:
Pulverize: the stem of Herba Cynomorii is pulverized, to obtain Songaria Cynomorium Herb;
Dry: Songaria Cynomorium Herb is dried, sieves;
Extraction: utilize supercritical CO2Songaria Cynomorium Herb after sieving is extracted by fluid, to obtain Herba Cynomorii oil
Extract;
Centrifugation: by Herba Cynomorii oil extract centrifugation, to obtain Herba Cynomorii oil.
The supercritical extraction process of a kind of Herba Cynomorii the most according to claim 1 oil, it is characterised in that
In extraction step, supercritical CO2The extracting pressure of fluid is 20MPa~30MPa, extraction temperature 35 DEG C~
45 DEG C, CO2Fluid flow is 12mL/min~20mL/min, and extraction time is 1.5h~2.5h.
The supercritical extraction process of a kind of Herba Cynomorii the most according to claim 2 oil, it is characterised in that
In extraction step, supercritical CO2The extracting pressure of fluid is 30MPa, extraction temperature 40 DEG C, CO2Fluid
Flow is 12mL/min, and extraction time is 2.5h.
The supercritical extraction process of a kind of Herba Cynomorii the most according to claim 2 oil, it is characterised in that
In extraction step, supercritical CO2The extracting pressure of fluid is 30MPa, extraction temperature 45 DEG C, CO2Fluid
Flow is 12mL/min, and extraction time is 2.5h.
The supercritical extraction process of a kind of Herba Cynomorii the most according to claim 2 oil, it is characterised in that
In extraction step, supercritical CO2The extracting pressure of fluid is 20MPa, extraction temperature 35 DEG C, CO2Fluid
Flow is 15mL/min, and extraction time is 1.5h.
The supercritical extraction process of a kind of Herba Cynomorii the most according to claim 2 oil, it is characterised in that
In extraction step, supercritical CO2The extracting pressure of fluid is 25MPa, extraction temperature 38 DEG C, CO2Fluid
Flow is 18mL/min, and extraction time is 1.8h.
The supercritical extraction process of a kind of Herba Cynomorii the most according to claim 2 oil, it is characterised in that
In extraction step, supercritical CO2The extracting pressure of fluid is 28MPa, extraction temperature 42 DEG C, CO2Fluid
Flow is 20mL/min, and extraction time is 2.2h.
8. according to the supercritical extraction process of a kind of Herba Cynomorii oil described in any one of claim 1~7, its feature
Being, in baking step, drying temperature is 30 DEG C~40 DEG C, and drying time is 18h~30h.
9. according to the supercritical extraction process of a kind of Herba Cynomorii oil described in any one of claim 1~7, its feature
Being, in pulverising step, the aperture of screen cloth is 0.177 μm~0.25 μm.
10., according to the supercritical extraction process of a kind of Herba Cynomorii oil described in any one of claim 1~7, it is special
Levying and be, in step with centrifugal separation, rotating speed is 10000r/min~12000r/min, the time of centrifugation
For 10min~30min.
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Cited By (2)
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CN106721742A (en) * | 2017-01-18 | 2017-05-31 | 范祖强 | A kind of many effect black garlic elite drinks and preparation method thereof |
CN109431869A (en) * | 2018-12-22 | 2019-03-08 | 南京益唯森生物科技有限公司 | A kind of cynomorium songaricum massage essential oil and preparation method thereof |
-
2016
- 2016-05-30 CN CN201610371077.9A patent/CN105861144A/en active Pending
Non-Patent Citations (1)
Title |
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危晴 等: "锁阳超临界萃取物成分的GC-MS分析", 《江苏农业科学》 * |
Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
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CN106721742A (en) * | 2017-01-18 | 2017-05-31 | 范祖强 | A kind of many effect black garlic elite drinks and preparation method thereof |
CN109431869A (en) * | 2018-12-22 | 2019-03-08 | 南京益唯森生物科技有限公司 | A kind of cynomorium songaricum massage essential oil and preparation method thereof |
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