CN106947583A - A kind of preparation method of raspberry seed oil and products thereof - Google Patents
A kind of preparation method of raspberry seed oil and products thereof Download PDFInfo
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- CN106947583A CN106947583A CN201710260464.XA CN201710260464A CN106947583A CN 106947583 A CN106947583 A CN 106947583A CN 201710260464 A CN201710260464 A CN 201710260464A CN 106947583 A CN106947583 A CN 106947583A
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- raspberry seed
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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
-
- 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
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- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Wood Science & Technology (AREA)
- Organic Chemistry (AREA)
- Medicines Containing Plant Substances (AREA)
- Acyclic And Carbocyclic Compounds In Medicinal Compositions (AREA)
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Abstract
The invention provides a kind of preparation method of raspberry seed oil and products thereof, including, pretreatment of raw material obtains raspberry seed fine powder；Entrainer is added, supercritical CO is carried out2Dynamic extraction, obtains raspberry seed oil；Wherein, the raspberry seed fine powder, its particle diameter is 400~600nm；Wherein, the entrainer, it is 1~5wt% polyglycerol ester solution.Raspberry seed oil product obtained by above-mentioned raspberry seed oil preparation method.Raspberry seed oil product obtained by the inventive method, it is on antioxygenic property, compared with other method, can 3 times of gain antioxidant effect.Polyglycerol ester entrainer of the present invention, in the range of preferred content, anthocyanidin can be extracted in 0.01~0.05% content range, stable microspheres solution system is then formed, and consolidate the enhancing for improving inoxidizability with the tocopherol in raspberry seed oil and other nutritional ingredients.
Description
Technical field
The invention belongs to oil and fat preparation technical field, and in particular to a kind of preparation method of raspberry seed oil and products thereof.
Background technology
Presently, supercritical extraction technique is a kind of new separation technology.It is facing using supercritical fluid as extractant
At boundary's temperature and pressure condition, the method that separation component is obtained from fluid or solid material.Using most extensive in food industry
Be supercritical CO2Extraction, it is to utilize CO2There is very high solvability to solute in the supercritical state, to realize to target
The extraction and separation of composition.
Compared with conventional method, oil yield made from traditional milling process is low, when carrying oil with organic solvent extractionprocess, again
The problems such as depositing dissolvent residual in the product, and it is low to produce efficiency.And supercritical CO2The oil product high income that fluid extraction is obtained, nothing
Problem of solvent residual.And this uses dynamic extraction, control reaction process can be observed at any time.
Raspberry is described as " gold fruit " in the international market, not only its pulp good mouthfeel, and tender succulence, fragrance is only
Spy, and contain substantial amounts of function factor.
Containing substantial amounts of unrighted acid and aliphatic acid needed by human especially in raspberry seed oil, its Linoleic acid,
The unsaturated fatty acid contents such as leukotrienes, oleic acid are higher.And contain many active materials in oil, such as tocopherol, phytosterol, many
Phenol etc., these active materials are widely used in the industries such as medicine, food, cosmetics because of its special property.But use conventional method
The tocopherol that measures, phytosterol, polyphenol, far away from utilizing supercritical CO2Dynamic extraction is high, because these materials is anti-oxidant
Poor-performing, easily decomposes or is converted into other material during liquefaction, greatly reduce the content of active material.
On the other hand, the raspberry seed oil obtained by prior art, the distinctive flower of its nutritional ingredient, especially raspberry seed
Blue or green element component, because it is hydrophilic molecule, not yet finds method, high efficiency extraction simultaneously stablizes survival in grease system.
The content of the invention
The purpose of this part is to summarize some aspects of embodiments of the invention and briefly introduce some preferably to implement
Example.It may do a little simplified or be omitted to avoid making our department in this part and the description of the present application summary and denomination of invention
Point, the purpose of specification digest and denomination of invention obscure, and this simplification or omit and cannot be used for limiting the scope of the present invention.
In view of technological gap prepared by above-mentioned and/or existing raspberry seed oil, it is proposed that the present invention.
Therefore, one of purpose of the invention is that there is provided a kind of raspberry seed oil for solution deficiency of the prior art
Preparation method.
In order to solve the above technical problems, the invention provides following technical scheme：Including pretreatment of raw material obtains raspberry
Seed fine powder；Entrainer is added, supercritical CO is carried out2Dynamic extraction, obtains raspberry seed oil；Wherein, the raspberry seed fine powder, its
Particle diameter is 400~600nm；Wherein, the entrainer, it is 1~5wt% polyglycerol ester solution.
As a kind of preferred scheme of the preparation method of raspberry seed oil of the present invention, wherein：The pretreatment of raw material,
It includes drying, and sieving is pulverized；1~5wt% polyglycerol esters solution, it is the ethanol of 1~5wt% polyglycerol esters
Solution.
As a kind of preferred scheme of the preparation method of raspberry seed oil of the present invention, wherein：The supercritical CO2It is dynamic
State is extracted, and its extracting pressure is 30~35MPa, and its extraction temperature is 35~45 DEG C.
As a kind of preferred scheme of the preparation method of raspberry seed oil of the present invention, wherein：The supercritical CO2It is dynamic
State is extracted, its extracting pressure, and it is 30Mpa.
As a kind of preferred scheme of the preparation method of raspberry seed oil of the present invention, wherein：The supercritical CO2It is dynamic
State is extracted, its extraction temperature, and it is 40 DEG C.
As a kind of preferred scheme of the preparation method of raspberry seed oil of the present invention, wherein：The supercritical CO2It is dynamic
State is extracted, its CO2Flow is 35~45g/min.
As a kind of preferred scheme of the preparation method of raspberry seed oil of the present invention, wherein：The supercritical CO2It is dynamic
State is extracted, its CO2Flow is 40g/min.
As a kind of preferred scheme of the preparation method of raspberry seed oil of the present invention, wherein：The extraction time, its
For 100min；The sieving, it was 400 mesh sieves；The drying, it is that drying to water content is 1~2%.
Another object of the present invention is that there is provided red obtained by a kind of preparation of above method for solution deficiency of the prior art
Raspberry seed oil product.
In order to solve the above technical problems, the invention provides following technical scheme：The raspberry seed oil, its contained insatiable hunger
It is 95~98% to account for total fatty acids ratio with aliphatic acid, and polyglycerol ester content is 1~2%, and anthocyanidin content is 0.01~0.05%.
Beneficial effects of the present invention：
Raspberry seed oil product obtained by the inventive method, it is on antioxygenic property, compared with other method, can 3 times of gain
Antioxidant effect.
Polyglycerol ester entrainer of the present invention, in the range of preferred content, can extract anthocyanidin 0.01~
0.05% content range, then forms stable microspheres solution system, and with the tocopherol in raspberry seed oil and other nutrition
Composition consolidates the enhancing for improving inoxidizability.
Embodiment
To enable the above objects, features and advantages of the present invention more obvious understandable, with reference to specific embodiment pair
The embodiment of the present invention is described in detail.
Many details are elaborated in the following description to fully understand the present invention, but the present invention can be with
It is different from other manner described here using other to implement, those skilled in the art can be without prejudice to intension of the present invention
In the case of do similar popularization, therefore the present invention is not limited by following public specific embodiment.
Secondly, " one embodiment " or " embodiment " referred to herein refers to may be included at least one realization side of the invention
Special characteristic, structure or characteristic in formula." in one embodiment " that different places occur in this manual not refers both to
Same embodiment, nor the single or selective embodiment mutually exclusive with other embodiment.
Embodiment 1：Sample preparation
Pretreatment of raw material
Dry, take raspberry seed, it is 1% to dry to water content；
Powder processed, 400 mesh sieves are crossed by raspberry seed, and grinding flour controls average grain diameter for 400nm.
Supercritical extract
Ethanol solution using 5wt% polyglycerol esters is as entrainer, and it is 30MPa to control extracting pressure, and temperature is 40 DEG C,
CO2Flow is 40g/min, extracts 100min.
Compound mensuration
Ultra Performance Liquid Chromatography-series connection quadrupole rod time-of-flight mass spectrometry (TOFMS) is used to determine anthocyanidin content to be specially
0.01%；
Use gas chromatography to determine unrighted acid and account for total fatty acids ratio for 98.00%；
Use in high effective liquid chromatography for measuring raspberry seed oil product containing polyglycerol ester as 1.00%.
Embodiment 2：Sample preparation
Pretreatment of raw material
Dry, take raspberry seed, it is 2% to dry to water content；
Powder processed, 200 mesh sieves are crossed by raspberry seed, and grinding flour controls average grain diameter for 500nm.
Supercritical extract
Acetone soln using 1wt% polyglycerol esters is as entrainer, and it is 30MPa to control extracting pressure, and temperature is 45 DEG C,
CO2Flow is 40g/min, extracts 100min.
Compound mensuration
Ultra Performance Liquid Chromatography-series connection quadrupole rod time-of-flight mass spectrometry (TOFMS) is used to determine anthocyanidin content to be specially
0.02%；
Use gas chromatography to determine unrighted acid and account for total fatty acids ratio for 97.70%；
Use in high effective liquid chromatography for measuring raspberry seed oil product containing polyglycerol ester as 1.10%.
Embodiment 3：Sample preparation
Pretreatment of raw material
Dry, take raspberry seed, it is 1% to dry to water content；
Powder processed, 400 mesh sieves are crossed by raspberry seed, and grinding flour controls average grain diameter for 600nm.
Supercritical extract
It is 30MPa to control extracting pressure, and temperature is 40 DEG C, CO2Flow is 40g/min, extracts 80min.
Compound mensuration
Determined, do not measured effectively dense in solution using Ultra Performance Liquid Chromatography-series connection quadrupole rod time-of-flight mass spectrometry (TOFMS)
The anthocyanidin of degree；
Use gas chromatography to determine unrighted acid and account for total fatty acids ratio for 97.00%；
Embodiment 4：Sample preparation
Pretreatment of raw material
Dry, take raspberry seed, it is 2% to dry to water content；
Powder processed, 200 mesh sieves are crossed by raspberry seed, and grinding flour controls average grain diameter for 200nm.
Supercritical extract
Ethanol solution using 2wt% polyglycerol esters is as entrainer, and it is 35MPa to control extracting pressure, and temperature is 45 DEG C,
CO2Flow is 35g/min, extracts 100min.
Compound mensuration
Ultra Performance Liquid Chromatography-series connection quadrupole rod time-of-flight mass spectrometry (TOFMS) is used to determine anthocyanidin content to be specially
0.02%；
Use gas chromatography to determine unrighted acid and account for total fatty acids ratio for 97.30%；
Use in high effective liquid chromatography for measuring raspberry seed oil product containing polyglycerol ester as 0.50%.
Embodiment 5：Sample preparation
Pretreatment of raw material
Dry, take raspberry seed, it is 1% to dry to water content；
Powder processed, 400 mesh sieves are crossed by raspberry seed, and grinding flour controls average grain diameter for 500nm.
Supercritical extract
It is 40MPa to control extracting pressure, and temperature is 20 DEG C, CO2Flow is 45g/min, extracts 120min.
Compound mensuration
Determined, do not measured effectively dense in solution using Ultra Performance Liquid Chromatography-series connection quadrupole rod time-of-flight mass spectrometry (TOFMS)
The anthocyanidin of degree；
Use gas chromatography to determine unrighted acid and account for total fatty acids ratio for 96.40%；
Embodiment 6：Sample preparation
Pretreatment of raw material
Dry, take raspberry seed, it is 8% to dry to water content；
Powder processed, 400 mesh sieves are crossed by raspberry seed, and grinding flour controls average grain diameter for 2000nm.
Supercritical extract
Ethanol solution using 10wt% polyglycerol esters is as entrainer, and it is 25MPa to control extracting pressure, and temperature is 60
DEG C, CO2Flow is 50g/min, extracts 120min.
Compound mensuration
Ultra Performance Liquid Chromatography-series connection quadrupole rod time-of-flight mass spectrometry (TOFMS) is used to determine anthocyanidin content to be specially
0.08%；
Use gas chromatography to determine unrighted acid and account for total fatty acids ratio for 86.05%；
Use in high effective liquid chromatography for measuring raspberry seed oil product containing polyglycerol ester as 2.80%.
Embodiment 7：Inoxidizability is tested
Antioxygen is determined using DPPH methods to the raspberry seed oil and anthocyanidin sample as obtained by above-mentioned embodiment 1,3,6
The property changed.
By the ethyl acetate dilution dissolving configuration sample liquid of raspberry seed oil samples obtained by embodiment 1,3,6.
Pipette ethyl acetate sample liquid extract solution respectively to mix with DPPH ethyl acetate solutions, room temperature dark place reaction 2h, then
It is withered with ethyl acetate solution blank in determining light absorption value under 517nm.With Trolox (water-soluble tocopherol) concentration to clearance rate
Make standard curve, calculate Trolox value antioxidation activities.As a result show that clearance rate is designated as R with a μm ol TE/100g oil meters.
R (%)=[1- (A2-A3)/A1] × 100%
A1-2.0mL DPPH ethyl acetate solution+2.0mL ethyl acetate solutions；
A2-2.0mL DPPH ethyl acetate solution+2.0mL oil sample acetic acid ethyl acetate extracts；
A3-2.0mL oil sample acetic acid ethyl acetate extract+2.0mL ethyl acetate solutions.
Concrete outcome such as table 7 below：
Table 7
| Embodiment 1 | Embodiment 3 | Embodiment 6 | Anthocyanidin |
| 89.80% | 50.04% | 65.56% | 23.01% |
From data in table 7, the polyglycerol ester selected in the present invention, anthocyanidin content can cooperate with enhancing raspberry
The antioxygenic property of seed oil.
Compared from the be the same as Example 3,6 of embodiment 1, raspberry seed oil made from my inventive method, it is in inoxidizability
It is stable to keep preferable effect on energy.
From the be the same as Example 6 of embodiment 1 compared to relatively, when raspberry seed size controlling is in 400~600nm, and will folder
Band agent content control matches other currently preferred technological parameters, can have good unsaturated fat at 1~5%
Acid content, anthocyanidin content.
From embodiment 1,3,6 and the experiment of the inoxidizability of anthocyanidin relatively, currently preferred particle diameter, entrainer
And other technological parameters, with synergy, more preferable antioxygenic property can be embodied.
Cashing for above-mentioned excellent effect, is because the present invention utilizes narrower polyglycerol ester content, pressure, temperature, stream
Amount, it is comprehensive to ensure effective extraction of anthocyanidin, and the anthocyanidin extracted is limited to narrower range simultaneously.Based on this, formed
Stable grease system containing hydrophily anthocyanidin, while ensureing the valid density of other nutrient molecules；And then so that anthocyanidin
With the nutrient molecules such as tocopherol synergy, strengthen inoxidizability.
To study and find through inventor, when Stress control is in 30~35Mpa, temperature is 35~45 DEG C, CO2 flows are 35~
During 45g/min, the concentration of the nutrient molecule such as tocopherol is just ensured.Temperature is too high, then nutrient molecule can be destroyed because of texture
And inactivate, temperature is too small, then causes that CO2 is mixed into the grease of collection again, makes it muddy.
Study and find through inventor, if pressure is excessive, flow is too small, because pressure is excessive, promote entrainment agent molecule whole
Tend to ordered arrangement in individual system, influence effective extraction concentration of entrainer, and then reduce extraction efficiency；If pressure is too small, stream
Amount is excessive, on the contrary because flow is excessive, has little time effectively extraction, equally reduces extraction efficiency.
Study and find through inventor, selected raspberry seed particle diameter is in 400~600nm, and it is on microcosmic because than table
The increase of area, can more preferably combine entrainer, if particle diameter is too small to have the generation of reunion situation, if particle diameter is excessive, can not have
The gain effect that nano effect is brought.And under specific temperature and pressure state, the raspberry seed fine powder of Nano grade can
Efficiently extract fuel-displaced.
Selected mass fraction of the invention is the ethanol solution of 1~5wt% polyglycerol ester, and it can efficiently extract on microcosmic
Hydrophilic anthocyanidin is taken, polyglycerol ester has hydrophilic and two kinds of groups of oleophylic simultaneously, and its content is controlled at 1~2%, being capable of shape
Into good microspheres solution, anthocyanidin is dynamically locked in polyglycerol ester microballoon, anthocyanidin and the tocopherol phase in grease
Mutually collaboration, can there is the synergy in terms of inoxidizability.
1~5wt% polyglycerol ester, the anthocyanidin content that it can be obtained by extraction is in the range of 0.01~0.02%, and two
Person be able to form stable microspheres solution system, if polyglycerol ester is too high, can cause that corresponding anthocyanidin content is too high simultaneously.It is poly- sweet
Grease is too high, can destroy the overall stable colloid state of raspberry seed oil, while so that anthocyanidin and tocopherol cooperate with chemistry
Balance is broken, and destroys final antioxygenic property.
It should be noted that the above embodiments are merely illustrative of the technical solutions of the present invention and it is unrestricted, although with reference to preferable
The present invention is described in detail embodiment, it will be understood by those within the art that, can be to technology of the invention
Scheme is modified or equivalent, and without departing from the spirit and scope of technical solution of the present invention, it all should cover in this hair
Among bright right.
Claims (10)
1. a kind of preparation method of raspberry seed oil, it is characterised in that：Including,
Pretreatment of raw material, obtains raspberry seed fine powder；
Entrainer is added, supercritical CO is carried out2Dynamic extraction, obtains raspberry seed oil；
Wherein, the raspberry seed fine powder, its particle diameter is 400~600nm；
Wherein, the entrainer, it is 1~5wt% polyglycerol ester solution.
2. the preparation method of raspberry seed oil as claimed in claim 1, it is characterised in that：The pretreatment of raw material, it is comprising dry
Dry, sieving is pulverized；
1~5wt% polyglycerol esters solution, it is the ethanol solution of 1~5wt% polyglycerol esters.
3. the preparation method of raspberry seed oil as claimed in claim 1 or 2, it is characterised in that：The supercritical CO2Dynamic extraction,
Its extracting pressure is 30~35MPa, and its extraction temperature is 35~45 DEG C.
4. the preparation method of raspberry seed oil as claimed in claim 1 or 2, it is characterised in that：The supercritical CO2Dynamic extraction,
Its extracting pressure, it is 30Mpa.
5. the preparation method of raspberry seed oil as claimed in claim 4, it is characterised in that：The supercritical CO2Dynamic extraction, its
Extraction temperature, it is 40 DEG C.
6. the preparation method of raspberry seed oil as claimed in claim 5, it is characterised in that：The supercritical CO2Dynamic extraction, its
CO2Flow is 35~45g/min.
7. the preparation method of raspberry seed oil as claimed in claim 5, it is characterised in that：The supercritical CO2Dynamic extraction, its
CO2Flow is 40g/min.
8. the preparation method of raspberry seed oil as any one of claim 5~7, it is characterised in that：The extraction time,
It is 100min；The sieving, it was 400 mesh sieves；The drying, it is that drying to water content is 1~2%.
9. a kind of raspberry seed oil by obtained by any one of the claims 1~8 raspberry seed oil preparation method is produced
Product.
10. a kind of raspberry seed oil as claimed in claim 9, it is characterised in that：The raspberry seed oil, its contained unsaturated lipid
It is 95~98% that fat acid, which accounts for total fatty acids ratio, and polyglycerol ester content is 1~2%, and anthocyanidin content is 0.01~0.05%.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2019128170A1 (en) * | 2017-12-28 | 2019-07-04 | 山东江天生物科技有限公司 | High-yield oil extraction method |
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| CN101891580A (en) * | 2010-07-05 | 2010-11-24 | 郑州大学 | Method for supercritical carbon dioxide extraction of lycopene in watermelon |
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Application publication date: 20170714 |