CN106821851B - A kind of fresh processing method of flos mume - Google Patents
A kind of fresh processing method of flos mume Download PDFInfo
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- CN106821851B CN106821851B CN201710090202.3A CN201710090202A CN106821851B CN 106821851 B CN106821851 B CN 106821851B CN 201710090202 A CN201710090202 A CN 201710090202A CN 106821851 B CN106821851 B CN 106821851B
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K8/00—Cosmetics or similar toiletry preparations
- A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
- A61K8/96—Cosmetics or similar toiletry preparations characterised by the composition containing materials, or derivatives thereof of undetermined constitution
- A61K8/97—Cosmetics or similar toiletry preparations characterised by the composition containing materials, or derivatives thereof of undetermined constitution from algae, fungi, lichens or plants; from derivatives thereof
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- A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
- A61K8/30—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds
- A61K8/49—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing heterocyclic compounds
- A61K8/4973—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing heterocyclic compounds with oxygen as the only hetero atom
- A61K8/498—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing heterocyclic compounds with oxygen as the only hetero atom having 6-membered rings or their condensed derivatives, e.g. coumarin
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- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61Q—SPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
- A61Q19/00—Preparations for care of the skin
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- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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- B01D11/02—Solvent extraction of solids
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Abstract
The invention discloses a kind of fresh processing method of flos mume, (1) freezing-extrusion wall-breaking: fresh flos mume, which is frozen into the frost flos mume of hard and squeezes, makes clasmatosis.(2) squeeze and extract separation: 0.5 times of -2 times of water is added in the flos mume of clasmatosis, stirs evenly, and squeezes separation cell liquid and flower slag.(3) flower slag extracts: concentration 20%-95% ethyl alcohol is added as solvent in gained flower slag, extraction is stirred at room temperature, obtain the flos mume extracting solution containing high-purity flavones.Flos mume fresh processing method whole process of the invention is energy-efficient without heating, and can be sufficiently reserved the effective component of flos mume, thermal instability substance recovery rate is significantly higher than the recovery rate of common dried flower;And technique continuity is good, obtains cell liquid and obtains spending slag simultaneously, simple extraction is not required to more purification steps and can be obtained the flos mume extract containing high-purity flavones;The flos mume cell liquid and flos mume extract product quality of acquisition are high, are widely portable to cosmetic field.
Description
Technical field
The invention mainly relates to cosmetic technical fields, specifically, the present invention relates to the fresh processing technique fields of flos mume.
Background technique
Flos mume also known as armeniaca mume are a kind of medicinal plum blossoms, are the bud of rose department plant plum Prunusmume, record
In " Chinese Pharmacopoeia ", have and open Yu Hezhong, the effect of resolving sputum, removing toxic substances, is used for gloomy vexed, stomachache due to emotional depression and the hyperactive liver-qi attacking the stomach, globus hysteriocus, cold ulcerative carbuncle
Poison etc..
Meanwhile in cosmetic field, flos mume also has long usage history, records in such as " pearl in red water " and " controls lip
The upper white plum valve of raw sore pastes it, such as cracks bleeder i.e. only." for another example " adopt precious collection " in record " plum blossom valve, snow-broth are cooked congee, relieving heat toxin,
Specialize in soothing liver-qi stagnation, the gorgeous body of beauty."
Flos mume mainly contains volatile oil, chlorogenic acid, flavonoids, the substances such as glycoside (Zhang Qinghua's flos mume chemical component
Research and bioactivity prerun [D] Shandong University, 2008.).According to Zhang Qinghua etc., flos mume Flavonoid substances, which have, to be inhibited
The activity of tyrosinase;Japanese scholars NakamuraS etc. reports the chlorogenic acid analog that flos mume contains, and has and inhibits black
Effect (NakamuraS, etc.Acylated sucroses and acylated the quinic acids of element production
analogsfrom theflower buds ofPrunus mume andtheirinhibitoryeffecton melanoge
nesis.Phytochemistry.2013Aug;92:128-36.) in recent years, the skin care function of flos mume is more excavated.
As Fang Zhaohua etc. with regard to the anti-carbonylation of armeniaca mume extract, facilitate fibrocyte proliferation, anti-sunlight function, applied for that invention is special
Sharp (CN104173220, CN104173221, CN104173222).
But the extraction processing method about flos mume, only a small number of prior arts.Xu Zhengdong etc. disclose it is a kind of from
The method (CN103330764) of extraction purification general flavone in flower bud of Japanese apricot, with dry flower bud of Japanese apricot, using refluxing extraction, in conjunction with big
Macroporous adsorbent resin isolation technics can quickly reach total flavonoid functional component extraction purification, total flavonoids substance in flower bud of Japanese apricot
To 80% or more content.Technology disclosed in Xu Zhengdong etc., mainly for the extraction of flavone compound.But flos mume is one
Kind of precious raw material, only 100 tons or so of annual output, in addition to flavone compound, flos mume also contains volatile oil, chlorogenic acid,
The ingredients such as chlorogenic acid analog, the patented technology could not make full use of other effective components, cause very big waste.
Importantly, the flos mume florescence is short, only 15 days or so;And flower is delicate, and storing and fresh-keeping is difficult.Therefore,
Peasant household is put into dry link after flos mume picking at once.In fresh flower drying process, the big portion of the fragrance matter of volatile oil
Divide loss, so being difficult to see the product that can retain flos mume fragrance in the market.
Meanwhile chlorogenic acid material stability is poor, degradation is easy in heating, During Illumination, and (such as woods Li Yang enhance green original
The West China technique study [J] the pharmaceutical journal of aqueous acid stability, 2005,20 (3): 225-227.).
If novel flos mume processing method can be developed, it is sufficiently reserved fragrance matter, chlorogenic acid, flavonoids etc., it will
It is of great immediate significance to the deep exploitation of flos mume.
Summary of the invention
For state of the art, especially existing flos mume processing method causes flos mume effective component that cannot integrate benefit
With, it is difficult to the status for retaining original fragrance matter, the present invention provides a kind of fresh processing methods of flos mume, using freezing, squeeze
Pressure technology, low-temp. extrusion extract flos mume cell liquid, have been sufficiently reserved the fragrance and unstable material of flos mume, and whole nothing
It needs to heat, low energy consumption;Clasmatosis is extracted, high-efficient;It squeezes and extracts remaining colored slag, ethanol-water solution is carried out as solvent
The Flavonoid substances that can be obtained high-purity are extracted, there is wide applicability in flos mume manufacture field.
To achieve the goals above, technical solution provided by the invention is as follows:
The present invention provides a kind of fresh processing method of flos mume, the processing method includes the following steps:
(1) freezing-extrusion wall-breaking: the flos mume of fresh picking is frozen into the frost flos mume of hard;Under freezing state
Hard flos mume is squeezed, and flos mume clasmatosis is made.
(2) squeeze and extract separation: water is added in the flos mume of clasmatosis, stirs evenly, and squeezes separation cell liquid and flower slag.
(3) flower slag extracts: ethanol-water solution is added as solvent in the flower slag of the flos mume obtained by step (2), is stirred at room temperature
It extracts, obtains flos mume extracting solution.
In the present invention, the pressing method, preferably screw are squeezed.
In the present invention, a kind of fresh processing method of flos mume is squeezed by twice: primary for squeezing after freezing
Cell wall, can be sufficiently destroyed by pressure, improve following process efficiency;It is primary to extract separation to squeeze, quick obtaining cell liquid, simultaneously
Colored slag is isolated, can be used as the extracting flavonoids raw material of next step.
In the present invention, the cell liquid that the step (2) obtains, definition is to be in fresh flos mume originally into the cell
Liquid destroys eucaryotic cell structure by freezing-wall-breaking method, water is added to squeeze the solution for extracting and obtaining.
In the present invention, the cell liquid that the step (2) obtains passes through centrifugation, film filtering, gelatin method, absorption, charging neutrality
Any one clarification technique in method, clarified cell liquid.
In the present invention, the flos mume cryogenic temperature of the fresh picking is -196 DEG C -- 10 DEG C.
Preferably, in the present invention, the flos mume cryogenic temperature of fresh picking is -30 DEG C -- 10 DEG C.
In the present invention, the amount of water before squeezing separation is 0.5 times -2 times of fresh flos mume quality.
In the present invention, the concentration of alcohol is 20%-95%.
In the present invention, the preferred 40%-80% of concentration of alcohol.
In the present invention, the flos mume extracting solution is further concentrated, dries, crushes, and obtains the flos mume rich in flavones and mentions
Take object powder.
The flos mume cell liquid of fresh processing method preparation or the flos mume extract rich in flavones of flos mume of the present invention exist
Application in cosmetics.
The flos mume cell liquid of fresh processing method preparation or the flos mume extract rich in flavones of flos mume of the present invention exist
Application in skin care solutions.
The flos mume cell liquid of fresh processing method preparation or the flos mume extract rich in flavones of flos mume of the present invention exist
Application in skin care emulsifier type.
Beneficial effects of the present invention:
A kind of fresh processing method of flos mume provided by the invention carries out after fresh flower picking using fresh flos mume as raw material
Freezing, the moisture of cell liquid are frozen into ice, and ice crystal can be such that flos mume cell wall fraction destroys;Flos mume after freezing carries out immediately
It squeezes, further promotes the broken of flos mume cell wall, so that effective component easily dissolves out.The wall-breaking method that the present invention uses is
Physical wall breaking without the use of other consumptive materials such as chemical reagent or enzymes, and can operate continuously, and low energy consumption, high-efficient.
Broken flos mume adds water to carry out extruding extraction, and Extracting temperature is low, high-efficient, the flos mume cell liquid tool of acquisition
There is strong flos mume fragrance;Low temperature extracts so that chlorogenic acid is adequately protected, so flos mume cell liquid contain it is a large amount of green
Ortho acid;Flos mume flower slag specific retention decline after freezing crushing, so that cell liquid yield significantly improves.
Since the cell in flos mume flower slag has been crushed, ethanol-water solution is added, is stirred at room temperature, can be obtained satisfaction
Recovery rate;And extraction process is squeezed, water-soluble carbohydrate etc. is separated from flos mume, but still containing there are many water-soluble
Property weaker ingredient, such as flavones, therefore flos mume flower slag adds ethanol-water solution extraction to can be obtained the white of the flavones containing high-purity
Aromatic substance, cell liquid, chlorogenic acid and general flavone in flos mume can be sufficiently separated extraction, mentioned significantly by Flos Mume extract
The high utilization rate of flos mume, is conducive to the flos mume resource for saving precious rareness.
Extracting method of the invention, whole process without heating, it is energy-efficient, and can be sufficiently reserved flos mume it is effective at
Point;The flos mume cell liquid and flos mume extract product quality of acquisition are high, are widely portable to provide in cosmetic field white
The fragrance and activity of plum blossom.It is of great immediate significance for the processing and use of flos mume.
Detailed description of the invention
Fig. 1 is shown as process flow of the invention.
Fig. 2 is shown as the cell liquid yield of different process.
Fig. 3 is shown as the cell fluid solid content of different process.
Fig. 4 is shown as the chlorogenic acid yield under different process.
Fig. 5 is shown as the general flavone purity under different process.
Fig. 6 is shown as the response surface figure that cryogenic temperature and amount of water influence chlorogenic acid yield.
Fig. 7 is shown as the response surface figure that cryogenic temperature and concentration of alcohol influence chlorogenic acid yield.
Fig. 8 is shown as the response surface figure that concentration of alcohol and amount of water influence chlorogenic acid yield.
Fig. 9 is shown as cryogenic temperature and amount of water to the response surface figure of general flavone impurities affect.
Figure 10 is shown as cryogenic temperature and concentration of alcohol to the response surface figure of general flavone impurities affect.
Figure 11 is shown as concentration of alcohol and amount of water to the response surface figure of general flavone impurities affect.
Specific embodiment
Specific embodiments of the present invention will be described in further detail below, but method of the invention is not limited to following realities
Apply example.
Fresh flos mume in the present invention, for the fresh petal that a bud just ready to burst, undried after picking, water content 70%-
93%;Flos mume dried flower, after referring to the picking of flos mume petal, the petal dried naturally, water content is lower than 15%;Chlorogenic acid,
Rutin standard items purity 98%;Screw-type extrusion device, high performance liquid chromatograph, ultraviolet-uisible spectrophotometer are conven-tional channels
Commercial equipment.
Embodiment one: the fresh processing method of flos mume
Referring to attached drawing 1, the present invention provides a kind of fresh processing method of flos mume, the processing method includes following step
It is rapid:
(1) freezing-extrusion wall-breaking: the flos mume of fresh picking is frozen into the frost flos mume of hard;Under freezing state
Hard flos mume is squeezed, and flos mume clasmatosis is made.
(2) squeeze and extract separation: water is added in the flos mume of clasmatosis, stirs evenly, and squeezes separation cell liquid and flower slag,
Calculate cell liquid yield, cell fluid solid content, chlorogenic acid yield.
(3) flower slag extracts: ethanol-water solution is added as solvent in the flower slag of the flos mume obtained by step (2), is stirred at room temperature
It extracts, obtains flos mume extracting solution, calculate chlorogenic acid yield general flavone purity.
Cell liquid yield=(cell liquid quality/fresh flos mume quality) * 100%.
Cell fluid solid content=((M3-M1)/M2) * 100%, M1 is container mass, and M2 is cell liquid quality, and M3 is cell
Together with the quality of container after liquid is dry;The test method of solid content are as follows: aluminium foil cup is weighed to obtain M1, takes solution quality M2 in aluminium foil
Cup, 105 DEG C of baking ovens, dry 3h, aluminium foil cup, which is placed in drier, to be cooled to room temperature, and weigh to obtain M3.
Chlorogenic acid yield=(extract Content of Chlorogenic Acid quality/material quality) * 100%, the material quality of fresh flos mume=
Actual mass * (1- fresh flower water content), material quality=actual mass * (1- dried flower water content) of flos mume dried flower;Chlorogenic acid
Test method is high performance liquid chromatography, and reference literature method is (green in white Yu .UV method and HPLC method measurement Chongqing region honeysuckle
Ortho acid and galuteolin comparision contents research [D] Southwest University, 2013.);Water content=((m1+m2-m3)/m1) * 100%;
Test method are as follows: take material quality m1, be placed in the container that quality is m2, in 105 DEG C of baking ovens, dry 3h is placed in drier
Be cooled to room temperature, weigh container and dry feedstock gross mass m3.
General flavone purity=(general flavone quality/extract quality) * 100%, test method are UV method, are pair with rutin
According to reference literature method (Zhang Qinghua's flos mume chemical constitution study and bioactivity prerun [D] Shandong University, 2008.).
Embodiment two: different processing methods cell liquid yield and solid content comparison
Referring to attached drawing 2 and attached drawing 3:
Technique 1: taking fresh flos mume 1Kg, -20 DEG C of freezing 12h, takes out and carries out screw attrition crushing, flos mume immediately
Flower mud adds 0.6Kg deionized water, stirs 5min;It carries out screw and squeezes extraction, acquired solution 3000rpm is centrifuged 5min, obtains clear
Clear white plum fresh flower cell liquid, is computed, and cell liquid yield is 75.2%, and cell fluid solid content is 3.0%.
Technique 2: taking fresh flos mume 1Kg, adds 0.6Kg deionized water, stirs 5min;It carries out screw and squeezes extraction, institute
It obtains solution 3000rpm and is centrifuged 5min, obtain clear white plum fresh flower cell liquid, be computed, cell liquid yield is 56.7%, cell liquid
Solid content is 1.8%.
Embodiment three: different processing methods chlorogenic acid yield
Referring to attached drawing 4:
Technique 3: fresh flos mume 1Kg (water content is 82.5% after tested) is taken, -20 DEG C of freezing 12h, taking-up carries out immediately
Screw attrition crushing, flos mume flower mud add 2Kg deionized water, stir 5min;It carries out screw and squeezes extraction, acquired solution
3000rpm is centrifuged 5min, obtains clear white plum fresh flower cell liquid, calculates after tested, and chlorogenic acid yield is 4.6% (with dry former
Material meter).
Technique 4: flos mume dried flower 200g (water content is 12.6% after tested) is taken, is crushed, is crossed 40 meshes, 2.8Kg is added to go
Ionized water boils rear slightly boiled extraction 1h;It carries out screw and squeezes extraction, acquired solution 3000rpm is centrifuged 5min, obtains clear white
Plum fresh flower cell liquid, calculates after tested, and chlorogenic acid yield is 3.1% (in terms of dry feedstock).
Example IV: different processing methods general flavone comparison or purity
Referring to attached drawing 5:
Technique 5: taking fresh flos mume 1Kg, -10 DEG C of freezing 12h, takes out and carries out screw attrition crushing, flos mume immediately
Flower mud adds 1Kg deionized water, stirs 5min;It carries out screw and squeezes extraction, 70% ethyl alcohol of 5L, room temperature is added in the flower slag of acquisition
2h is stirred, flos mume extracting solution is filtered to obtain, 60 DEG C are concentrated under reduced pressure, are freeze-dried to obtain the flos mume extract rich in flavones;Through examining
It surveys, general flavone purity is 57.1% in the extract.
Technique 6: taking fresh flos mume 1Kg, carries out screw attrition crushing, and 70% ethyl alcohol of 5L, room is added in flos mume flower mud
Temperature stirring 2h, filters to obtain flos mume extracting solution, and 60 DEG C are concentrated under reduced pressure, are freeze-dried to obtain flos mume extract;Through detecting, the extraction
General flavone purity is 18.0% in object.
Technique 7: taking flos mume dried flower 200g, crushes, and crosses 40 meshes, and 800ml water, 70% ethyl alcohol of 5L, refluxing extraction is added
2h filters to obtain flos mume extracting solution, and 60 DEG C are concentrated under reduced pressure, are freeze-dried to obtain flos mume extract;It is total in the extract through detecting
Flavones purity is 20.7%.
Technique 8: taking flos mume dried flower 200g, crushes, and crosses 40 meshes, and 800ml water, 70% ethyl alcohol of 5L, refluxing extraction is added
2h, filters to obtain flos mume extracting solution, and 60 DEG C are concentrated under reduced pressure into 600g, is added 500g D101 resin, Static Adsorption 12h, 2L go from
Sub- water washing resin, resin 80% ethanol elution of 3L after washing collect eluent;60 DEG C of eluent are concentrated under reduced pressure, freeze
Dry flos mume extract;Through detecting, general flavone purity is 60.2% in the extract.
Extracting method (technique 5) of the present invention, general flavone purity are 57.1%, and purity is close to macroporous resin purification
General flavone purity 60.2%, is significantly higher than technique 6 (18.0%) and technique 7 (20.7%) obtained by extracting method (technique 8), referring to
Figure of description 5;More importantly extracting method of the present invention is not necessarily to subsequent purification process, that is, can reach similar macropore
The general flavone purity of purifying resin, is not required to other materials and reagent, and discharging of waste liquid is few, high-efficient.
Embodiment five: response phase method optimizes processing method of the present invention
The fresh flos mume of multiple groups 1Kg is weighed respectively, it is hard to quality according to the method for the invention freezing 12h, it squeezes broken
It is broken, add deionized water, stir 5min, screw, which squeezes, to be extracted, and the flower slag and cell liquid of acquisition are detected and calculated in cell liquid
Chlorogenic acid yield;5L ethanol-water solution is added in flower slag, and 2h is stirred at room temperature, filters to obtain flos mume extracting solution, 60 DEG C be concentrated under reduced pressure,
It is freeze-dried to be rich in the flos mume extract of flavones;It detects and calculates general flavone purity in the extract.
Response phase method is as follows to the optimization process of above-mentioned technological parameter:
Table 1: response surface factor level table
Process conditions | Unit | Minimum value | Maximum value |
Cryogenic temperature | ℃ | -30 | -10 |
Amount of water | Times | 0.5 | 2 |
Concentration of alcohol | % | 20 | 95 |
Chlorogenic acid yield | % | Response | 0.10556 |
AlwaysIt is yellowKetone is pureDegree | % | Response | 1.97238 |
The influence of cryogenic temperature, amount of water and concentration of alcohol to chlorogenic acid yield and general flavone purity of the present invention.
Table 2:Box-bohnken experimental design result
Response phase method optimizes experimental result, referring to attached drawing 6-11 it is found that cryogenic temperature, amount of water and concentration of alcohol are to this hair
Bright chlorogenic acid yield and general flavone impurities affect all have conspicuousness, and cryogenic temperature, amount of water and concentration of alcohol are to green original
The effect tendency of sour yield and general flavone purity is slightly different.Optimal combination be -20 DEG C of cryogenic temperature, amount of water be 1.25 times
Fresh flos mume quality and concentration of alcohol 57.5%, obtain chlorogenic acid yield and general flavone purity highest, can achieve chlorogenic acid
Yield 5.0% or so, general flavone purity is 58% or so.
Embodiment six: the preparation of flos mume cell liquid and the flos mume extract rich in flavones
Fresh flos mume 1Kg, -20 DEG C of freezing 8h are taken, takes out and carries out screw attrition crushing immediately, flos mume flower mud adds
1Kg deionized water stirs 5min;It carries out screw and squeezes extraction, obtain flos mume cell liquid and flos mume flower slag.
Gained flos mume cell liquid is centrifuged 10min through 4000rpm, obtains clear white plum fresh flower cell liquid, through detecting, cell
Fluid solid content is 2.6%, and chlorogenic acid yield is 4.8%, with strong flos mume fragrance;White plum fresh flower cell liquid can be applied to
All dosage forms of cosmetics;
80% ethyl alcohol of 4L is added in flos mume flower slag, and 2h is stirred at room temperature, filters to obtain flos mume extracting solution, 60 DEG C be concentrated under reduced pressure,
It is freeze-dried to be rich in the flos mume extract of flavones;Through detecting, general flavone purity is 57.6% in the extract;Rich in flavones
Flos mume extract can be applied to all dosage forms of cosmetics.
Embodiment seven: the preparation of flos mume cell liquid and the flos mume extract rich in flavones
Fresh flos mume 1Kg, -30 DEG C of freezing 8h are taken, takes out and carries out screw attrition crushing immediately, flos mume flower mud adds
0.5Kg deionized water stirs 5min;It carries out screw and squeezes extraction, obtain flos mume cell liquid and flos mume flower slag.
Gained flos mume cell liquid is centrifuged 10min through 4000rpm, obtains clear white plum fresh flower cell liquid, through detecting, cell
Fluid solid content is 3.4%, and chlorogenic acid yield is 4.4%, with strong flos mume fragrance;White plum fresh flower cell liquid can be applied to
All dosage forms of cosmetics;
20% ethyl alcohol of 4L is added in flos mume flower slag, and 2h is stirred at room temperature, filters to obtain flos mume extracting solution, 60 DEG C be concentrated under reduced pressure,
It is freeze-dried to be rich in the flos mume extract of flavones;Through detecting, general flavone purity is 46.6% in the extract;Rich in flavones
Flos mume extract can be applied to all dosage forms of cosmetics.
Embodiment eight: the preparation of flos mume cell liquid and the flos mume extract rich in flavones
Fresh flos mume 1Kg, -10 DEG C of freezing 8h are taken, takes out and carries out screw attrition crushing immediately, flos mume flower mud adds
2Kg deionized water stirs 5min;It carries out screw and squeezes extraction, obtain flos mume cell liquid and flos mume flower slag.
Gained flos mume cell liquid is centrifuged 10min through 4000rpm, obtains clear white plum fresh flower cell liquid, through detecting, cell
Fluid solid content is 1.6%, and chlorogenic acid yield is 4.1%, with strong flos mume fragrance;White plum fresh flower cell liquid can be applied to
All dosage forms of cosmetics;
95% ethyl alcohol of 4L is added in flos mume flower slag, and 2h is stirred at room temperature, filters to obtain flos mume extracting solution, 60 DEG C be concentrated under reduced pressure,
It is freeze-dried to be rich in the flos mume extract of flavones;Through detecting, general flavone purity is 48.7% in the extract;Rich in flavones
Flos mume extract can be applied to all dosage forms of cosmetics.
Embodiment nine: the preparation of flos mume cell liquid and the flos mume extract rich in flavones
Fresh flos mume 1Kg, -15 DEG C of freezing 8h are taken, takes out and carries out screw attrition crushing immediately, flos mume flower mud adds
1.25Kg deionized water stirs 5min;It carries out screw and squeezes extraction, obtain flos mume cell liquid and flos mume flower slag.
Gained flos mume cell liquid is centrifuged 10min through 4000rpm, obtains clear white plum fresh flower cell liquid, through detecting, cell
Fluid solid content is 2.8%, and chlorogenic acid yield is 4.7%, with strong flos mume fragrance;White plum fresh flower cell liquid can be applied to
All dosage forms of cosmetics;
4L40% ethyl alcohol is added in flos mume flower slag, and 2h is stirred at room temperature, filters to obtain flos mume extracting solution, 60 DEG C be concentrated under reduced pressure,
It is freeze-dried to be rich in the flos mume extract of flavones;Through detecting, general flavone purity is 55.7% in the extract;Rich in flavones
Flos mume extract can be applied to all dosage forms of cosmetics.
Embodiment ten: the preparation of flos mume cell liquid and the flos mume extract rich in flavones
Fresh flos mume 1Kg is taken, container is loaded on, is placed in liquid nitrogen container (- 196 DEG C) 15min, progress screw immediately is taken out and squeezes
Crush broken, flos mume flower mud adds 1.25Kg deionized water, stirs 5min;It carries out screw and squeezes extraction, obtain flos mume cell
Liquid and flos mume flower slag.
10ml0.05% chitosan solution is added in gained flos mume cell liquid, stirs 15min, is centrifuged through 4000rpm
10min obtains clear white plum fresh flower cell liquid, and through detecting, cell fluid solid content is 2.7%, and chlorogenic acid yield is 4.6%, tool
There is strong flos mume fragrance;White plum fresh flower cell liquid can be applied to all dosage forms of cosmetics;
50% ethyl alcohol of 4L is added in flos mume flower slag, and 2h is stirred at room temperature, filters to obtain flos mume extracting solution, 60 DEG C be concentrated under reduced pressure,
It is freeze-dried to be rich in the flos mume extract of flavones;Through detecting, general flavone purity is 56.6% in the extract;Rich in flavones
Flos mume extract can be applied to all dosage forms of cosmetics.
Embodiment 11: the preparation of flos mume cell liquid and the flos mume extract rich in flavones
Fresh flos mume 1Kg is taken, container is loaded on, -80 DEG C of freezing 1h take out and carry out screw attrition crushing, Bai Mei immediately
Flower flower mud adds 1.25Kg deionized water, stirs 5min;It carries out screw and squeezes extraction, obtain flos mume cell liquid and flos mume flower
Slag.
10ml0.05% chitosan solution is added in gained flos mume cell liquid, stirs 15min, is centrifuged through 4000rpm
10min obtains clear white plum fresh flower cell liquid, and through detecting, cell fluid solid content is 2.8%, and chlorogenic acid yield is 4.7%, tool
There is strong flos mume fragrance;White plum fresh flower cell liquid can be applied to all dosage forms of cosmetics;
50% ethyl alcohol of 4L is added in flos mume flower slag, and 2h is stirred at room temperature, filters to obtain flos mume extracting solution, 60 DEG C be concentrated under reduced pressure,
It is freeze-dried to be rich in the flos mume extract of flavones;Through detecting, general flavone purity is 57.1% in the extract;Rich in flavones
Flos mume extract can be applied to all dosage forms of cosmetics.
Embodiment 12: the preparation of flos mume cell liquid and the flos mume extract rich in flavones
Fresh flos mume 1Kg is taken, container is loaded on, is placed in -40 DEG C of freezing 2h, takes out and carries out screw attrition crushing immediately,
Flos mume flower mud adds 1.25Kg deionized water, stirs 5min;It carries out screw and squeezes extraction, obtain flos mume cell liquid and Bai Mei
Spend colored slag.
10ml0.05% chitosan solution is added in gained flos mume cell liquid, stirs 15min, is centrifuged through 4000rpm
10min obtains clear white plum fresh flower cell liquid, and through detecting, cell fluid solid content is 2.6%, and chlorogenic acid yield is 4.8%, tool
There is strong flos mume fragrance;White plum fresh flower cell liquid can be applied to all dosage forms of cosmetics;
50% ethyl alcohol of 4L is added in flos mume flower slag, and 2h is stirred at room temperature, filters to obtain flos mume extracting solution, 60 DEG C be concentrated under reduced pressure,
It is freeze-dried to be rich in the flos mume extract of flavones;Through detecting, general flavone purity is 57.4% in the extract;Rich in flavones
Flos mume extract can be applied to all dosage forms of cosmetics.
Embodiment 13: flos mume cell liquid facial treatment essence
Table 3: flos mume cell liquid facial treatment essence
Preparation method: sodium alginate and hyaluronic acid are dispersed in water 60min, other compositions are added, are sufficiently dissolved as A
Phase;B phase is added after stirring evenly, stirs evenly up to flos mume cell liquid facial treatment essence.
Embodiment 14: flos mume skin cream
Table 4: flos mume skin cream
Preparation method: being dispersed in water 60min for sodium alginate, and other compositions are added, and stirring is sufficiently dissolved as A phase;Separately
The all the components weighed in B phase are uniformly mixed;B is added in A phase, homogeneous 5 minutes, C phase is added, stirred evenly up to flos mume
Skin cream.
Flos mume first freeze acquisition frost flos mume, before not melting, squeezed immediately, it can be achieved that cell wall it is abundant
It is broken;This method is simple and efficient, and low energy consumption;The flos mume flower mud obtained after broken wall can carry out immediately after adding water and stirring uniformly
It squeezes and extracts, the operating time is short, and temperature is low, can retain the determination system of thermal unstable material such as fragrance and the chlorogenic acid of flos mume;Extraction
The remaining colored slag of flos mume cell liquid still containing the ingredient weaker there are many water solubility, such as flavones, therefore can be used as flos mume Huang
The extraction raw material of ketone, makes full use of flos mume medicinal material;And squeeze to extract and displaced significant portion of non-Flavonoid substances,
So that flower slag adds alcohol-water to extract, other purification steps are not necessarily to, can be obtained the flos mume extract containing high-purity flavones;
Integrated artistic is coherent, strong operability, high-efficient and low energy consumption in the process, discharging of waste liquid is few, is suitble to industrialized production.
As described above, the present invention can be realized preferably, the above embodiments are only to preferred implementation side of the invention
Formula is described, and is not intended to limit the scope of the present invention, and without departing from the spirit of the design of the present invention, this field is common
The various changes and improvements that technical staff makes technical solution of the present invention, should all fall into present invention determine that protection scope in.
Claims (6)
1. a kind of fresh processing method of flos mume, which is characterized in that the processing method includes the following steps:
(1) freezing-extrusion wall-breaking: the flos mume of fresh picking, -30 DEG C of cryogenic temperature -- 10 DEG C of white plums of frost for being frozen into hard
Flower;Hard flos mume under freezing state is squeezed, and flos mume clasmatosis is made;
(2) squeeze and extract separation: 0.5 times of -2 times of water of fresh flos mume quality are added in the flos mume of clasmatosis, stir evenly, and squeeze
Pressure separation cell liquid and flower slag;
(3) flower slag extracts: it is 20%-95% ethanol water as solvent that concentration is added in the flower slag of the flos mume obtained by the step (2),
Extraction is stirred at room temperature, obtains flos mume extracting solution.
2. a kind of fresh processing method of flos mume as described in claim 1, which is characterized in that the pressing method, preferably
Screw squeezes.
3. a kind of fresh processing method of flos mume as described in claim 1, which is characterized in that the step (2) squeezes separation
The cell liquid of acquisition passes through any one clarification technique in centrifugation, film filtering, gelatin method, absorption, charge neutralization, clarification
Cell liquid.
4. a kind of fresh processing method of flos mume as described in claim 1, which is characterized in that the flos mume extracting solution is into one
Step concentration, dry, crushing, obtain the flos mume extract powder rich in flavones.
5. a kind of fresh processing method of flos mume as described in claim 1, which is characterized in that optimizing technology parameters: fresh to adopt
The flos mume cryogenic temperature plucked is -20 DEG C, and 1.25 times of amount of water, the concentration of ethanol-water solution is 57.5%.
6. the flos mume cell liquid of the fresh processing method preparation of a kind of flos mume as claimed in claim 4 or rich in the white of flavones
Application of the Flos Mume extract in cosmetics.
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CN101978974A (en) * | 2010-10-20 | 2011-02-23 | 汤永强 | Method for extracting bioactive substance by breaking walls of chlorella pyrenoidosa chick |
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CN101978974A (en) * | 2010-10-20 | 2011-02-23 | 汤永强 | Method for extracting bioactive substance by breaking walls of chlorella pyrenoidosa chick |
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