CN109430371A - A kind of ginseng fructus lycii Ultramicro-powder microwave vacuum freeze drying means - Google Patents
A kind of ginseng fructus lycii Ultramicro-powder microwave vacuum freeze drying means Download PDFInfo
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- CN109430371A CN109430371A CN201811310287.2A CN201811310287A CN109430371A CN 109430371 A CN109430371 A CN 109430371A CN 201811310287 A CN201811310287 A CN 201811310287A CN 109430371 A CN109430371 A CN 109430371A
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- fructus lycii
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- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23B—PRESERVING, e.g. BY CANNING, MEAT, FISH, EGGS, FRUIT, VEGETABLES, EDIBLE SEEDS; CHEMICAL RIPENING OF FRUIT OR VEGETABLES; THE PRESERVED, RIPENED, OR CANNED PRODUCTS
- A23B7/00—Preservation or chemical ripening of fruit or vegetables
- A23B7/02—Dehydrating; Subsequent reconstitution
- A23B7/024—Freeze-drying, i.e. cryodessication or lyophilisation
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- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23B—PRESERVING, e.g. BY CANNING, MEAT, FISH, EGGS, FRUIT, VEGETABLES, EDIBLE SEEDS; CHEMICAL RIPENING OF FRUIT OR VEGETABLES; THE PRESERVED, RIPENED, OR CANNED PRODUCTS
- A23B7/00—Preservation or chemical ripening of fruit or vegetables
- A23B7/04—Freezing; Subsequent thawing; Cooling
Abstract
The invention discloses a kind of ginseng fructus lycii Ultramicro-powder microwave vacuum freeze drying means, includes the following steps: 1) to pre-process: by the ginseng of fresh harvesting, fructus lycii, silt is eluted with water, drains；2) it is beaten: pretreated ginseng, fructus lycii and water three is beaten；3) it is concentrated: slurries is turned to be concentrated through reverse osmosis unit；4) precooling: the concentrate being concentrated through reverse osmosis unit is stirred with high-speed mixer, is then freezed；5) it is freeze-dried: Cryo-concentration liquid is put into dryness storehouse, carry out vacuum freeze drying, dried and taken out after bleeding off pressure from dryness storehouse；6) it crushes: being crushed with airslide disintegrating mill to get fructus lycii ginseng submicron powder.Method of the invention effectively reduces freeze-drying time, reduces energy consumption of freeze drying, remains active constituent, effective component, maintains the good rehydration of product.
Description
Technical field
The present invention relates to a kind of drying means of ginseng fructus lycii more particularly to a kind of ginseng fructus lycii Ultramicro-powder microwave vacuum are cold
Drying method is lyophilized.
Background technique
The name of fructus lycii is said in Compendium of Material Medica first appeared in Shennong's Herbal, drug scholar's Li Shizhen (1518-1593 A.D.) of the Ming Dynasty: " Chinese holly
Qi, two tree names.The thorn of this object spine such as Chinese holly, the item of stem such as Qi, therefore and name it.Long term usage heavily fortified point muscles and bones is made light of one's life by commiting suicide not old, resistance to cold and heat.Mend essence
Unsaturated vapor, beauty treatment, skin bleach, improving eyesight and quiet nerves, make us long-lived." fructus lycii sweet taste benefit, spring can be same with the product of tepor sweet in flavor
When take, yang-energy hair tonic of helping others.Summer compatibility chrysanthemum can remove irascibility with enriching yin improving eyesight.Autumn eats fructus lycii and needs with moist food
Product, such as pyrus nivalis, tendril-leaved fritillary bulb, radix polygonati officinalis etc., effect is more preferable.Winter fructus lycii can flat yang-tonifying gas, facilitate human body growth, resist
Nature severe cold.Fructus lycii is the Chinese medicine for having fine development prospect simply, should further widen its research field from now on, is sufficiently sent out
Its health care and medical value are waved, is allowed to preferably as mankind's health service.
Ginseng comes from " book on Chinese herbal medicine ".Ginseng: shape is long and yellow, shape such as radix saposhnikoviae, Duo Runshi and it is sweet, custom is heavy Paekche with not entering to take
Person, shape is thin and hard white, and smell is thinner than Shangdang；Secondary to use Koryo, shape is big and empty soft, not as good as Paekche, practical and too late Shangdang person.Ancient times
The refined of ginseng is known as rhizoma polygonati, Goblin, god grass.Ginseng is known as " King of Herbs ", is well-known " northeast Triratna " (people
Ginseng, fur, pilose antler) one of, be have won fame both at home and abroad, the rare medicinal herbs that old children all knows.
Ginseng reinforces vital energy, reinforces the spleen to benefit the lung, the beneficial blood that promotes the production of body fluid, calming the nerves increases intelligence, nourishing and strengthening Yin and Yang, adjust balance, improve
The effect of immunity；Fructus lycii has the effect of nourishing liver and kidney, improving eyesight, beneficial complexion, long muscle, hard muscles and bones.Papillary long term usage, which has, prolongs
Year lengthens one's life, the effect of anti-aging.
Freeze Drying Technique is much studied and is reported in the application of the dry processing of fructus lycii at present, it with dry, hot wind
The fructus lycii of seasoning production is compared, not only the effective components such as polysaccharide, glycine betaine, carotenoid, flavones, amino acid and thermal sensitivity
Ingredient etc. is not damaged, and can keep color, nutritional ingredient, appearance and the active material of fresh goods to the maximum extent.Than
Such as: number of patent application: 201410215617.5, a kind of preparation method that fructus lycii is lyophilized is disclosed, is operated as follows:
(1) it prepares composite edible aqueous slkali: preparing mixed solution with sodium carbonate and potassium carbonate, wherein the quality of sodium carbonate and potassium carbonate
Concentration is respectively 50%, then mixed solution pH value is adjusted to 8~9 to get composite edible aqueous slkali；(2) fructus lycii is put into compound
It impregnates in edible alkali solution, weight ratio=1:1~1.5 of fructus lycii and composite edible aqueous slkali, after impregnating 30~50 minutes, picks up
Draining is cleaned to fructus lycii surface pH value=7, draining with drinking water, weighs sabot；(3) under conditions of 0 37~subzero 39 DEG C,
Freeze 4~6 hours；(4) fructus lycii after freezing carries out vacuum freeze drying processing, and export is got product；In step (4),
Vacuum freeze drying processing technical parameter require it is as follows: vacuum degree: first 15 hours be 110~180Pa, 16 hours~21 hours
For 80~90Pa, 22 hours~32 hours are 40~60Pa；Temperature of heating plate: subzero 10 DEG C, 6 hours → 5 DEG C are maintained, maintains 6
Hour → 10 DEG C, 3 hours → 20 DEG C are maintained, maintains 3 hours → 40 DEG C, maintains 3 hours → 60 DEG C, maintains 3 hours → 80 DEG C, dimension
3 hours → 70 DEG C are held, maintains 3 hours → 55 DEG C, is maintained 2 hours；Condenser temperature: subzero 38~42 DEG C subzero.Number of patent application:
201510985260.3, a kind of processing method that fructus lycii is lyophilized is disclosed, this method presses step (5) vacuum freeze drying: will
To medlar fresh fruit uniformly, single layer be layered on stainless steel freeze-drying pallet in, put into the drying box of freeze drier, when material temperature
When degree reaches -35 DEG C or less, vacuum pump is opened, after maintaining 120~360min, temperature programming, temperature-rise period are carried out to partition
Are as follows: temperature cools to -45 DEG C~-35 not higher than -35 DEG C of holding 2h → being warming up to -25 DEG C~-20 DEG C holding 2.5-3 .5h →
DEG C 2h → be warming up to -15 DEG C~-10 DEG C holding 2.5-3.5h → cooling to -25~-20 DEG C of holding 4h → is kept to be warming up to 25
DEG C keep 8h, be warming up to 40 DEG C of -45 DEG C of holding 12h, control moisture≤5% of final products.Number of patent application:
201510985259.0, the freeze-drying processing method of fructus lycii magma is disclosed, this method is lyophilized by step (4): the Chinese holly that will have been squeezed the juice
Qi is put into freeze dryer, and pre-freeze is carried out at -20~0 DEG C, and the pre-freeze time is 1~2 hour, continues to be cooled to temperature to be -35 DEG C
~-30 DEG C, freeze-drying time is 12~14 hours, and gradient increased temperature is taken in heating, and the time of heating is 10~12 hours, final to parse
Temperature is 30~45 DEG C, and parsing pressure is 40~60Pa.
However, these vacuum freeze-drying technique sublimation dryings are all very long, energy consumption is big, and the production cycle is long, system
The about industrialized production of Freeze Drying Technique.Freeze-drying time could be saved when in some methods by being cut into very thin thickness,
But yield just declines, and specific energy consumption is increased by.
Fructus lycii is squeezed the juice in certain methods or filters out juice after adding water mashing, with regard to taking juice to be freeze-dried, is not had
Accomplish full nutritional utilization wolfberry, cause fructus lycii utilization rate relatively low, and when vacuum freeze-drying technique freeze-drying
Between it is also very long.Number of patent application: 201410499073.X discloses the preparation method of the fresh juicing powder of vacuum freezing-dried wolfberry,
Step (1) pre-freeze: the fresh juicing sabot of fructus lycii is paved, freezing chamber carry out slow freezing, pre-freeze condition are as follows: sabot amount be 5~
10kg/m2, material thickness is 2~3cm, and pre-freezing temperature is -30 DEG C to -35 DEG C, and the pre-freeze time is 10-16h；Step (2) distillation
It is dry: the good material of pre-freeze being put into the dryness storehouse of vacuum freeze-drying machine, cold distillation is carried out, sets work pressure during lyophilization
Power is 3-30Pa, and lyophilization temperature is 25-40 DEG C, condenser temperature is -40 to -60 DEG C, lyophilization time 8-12h；Step
(3) parsing-desiccation is carried out to the material after step (2) lyophilization, operating pressure is 20-30Pa, desorption during desorbing and drying
Drying temperature is 60-80 DEG C, and the desorbing and drying time is 1-3h；(4) crushing packet is carried out to the material after step (3) parsing-desiccation
Dress.
To solve drawbacks described above, there is higher cost for vacuum freeze drying, the production cycle is long, and big wait of specific energy consumption lacks
Point, inventor have carried out a large amount of research work, propose a kind of new preparation method.
Summary of the invention
Present invention aims to overcome that the shortcomings of the prior art, proposes a kind of energy rapid microwave vacuum freeze drying people
The method for joining fructus lycii Ultramicro-powder shortens the production cycle being entirely lyophilized, and specific energy consumption and cost, which is lyophilized, to be reduced, but also sufficiently
New fresh fructus lycii, the effective component of ginseng, nutritional ingredient are kept, product rehydration obtained is high, its color, quality after adding water to restore
Do not have difference substantially with fresh goods.
To achieve the goals above, present invention employs technique below and steps:
A kind of ginseng fructus lycii Ultramicro-powder microwave vacuum freeze drying means, method includes the following steps:
1. a kind of ginseng fructus lycii Ultramicro-powder microwave vacuum freeze drying means, it is characterised in that this method includes the following steps:
1) it pre-processes: by the ginseng of fresh harvesting, fructus lycii, silt is eluted with water, drains；
2) it is beaten: being 1:0.5~2:2~10 by pretreated ginseng, fructus lycii and water proportions, be put into high-speed shearing machine progress
Mashing；
3) it is concentrated: the slurries of step 2 is turned through reverse osmosis unit, reverse osmotic pressure is 0.1~4.0MPa, controls reverse osmosis membrane filtration
Excess temperature is 0~30 DEG C, and running to the partial volume that shuts off is the 10~40% of total volume, takes out concentrate；
4) precooling: the concentrate that step 3) is concentrated through reverse osmosis unit -10~0 DEG C at a temperature of, use high-speed mixer
It is stirred, is passed through gas while stirring, be allowed to become porous material；The then pre-freeze 0.5~2 at -30~-35 DEG C
Hour, guarantee that concentrate sufficiently freezes；
5) it is freeze-dried: the cold well temperature of dryness storehouse being first down to -35 DEG C hereinafter, being then put into step 4) Cryo-concentration liquid
In dryness storehouse, dryness storehouse is vacuumized, vacuum degree opens microwave generator control microwave power 100 after reaching 20~100Pa
~200w makes temperature of charge rise to -15~-20 DEG C from -30~-35 DEG C in 3~4 hours；Adjust the microwave of microwave generator
Power makes temperature of charge rise to 0 DEG C from -15~-20 DEG C to 200~300w in 2~3 hours；Microwave generator is adjusted again
Microwave power makes temperature of charge rise to 30 DEG C from 0 DEG C to 300~400w in 1~2 hour, takes out after bleeding off pressure from dryness storehouse,
Obtaining biodiversity content is 5% freeze-drying prods below；
6) it crushes: being 5% freeze-drying prods below by biodiversity content after vacuum freeze drying, use air-flow powder at 30 DEG C or less
Broken machine is crushed, so that 95% or more grain size of micropowder reaches 15 μm hereinafter, up to ginseng fructus lycii Ultramicro-powder；
7) it packs: ginseng fructus lycii Ultramicro-powder is fitted into clean packaging, airtight vacuum or rush nitrogen and pack.
Preferably, step 4) are as follows: the concentrate that step 3) is concentrated through reverse osmosis unit -10~0 DEG C at a temperature of, use
High-speed mixer is stirred, and is passed through nitrogen while stirring, and is allowed to become porous material, porosity to 25%；Then
Pre-freeze 1 hour at -30~-35 DEG C guarantees that concentrate sufficiently freezes.
Preferably, step 5) are as follows: the cold well temperature of dryness storehouse is first down to -35 DEG C hereinafter, then by step 4) precooling
Concentrate is put into dryness storehouse, is vacuumized to dryness storehouse, and vacuum degree opens microwave generator control microwave after reaching 20~100Pa
Power makes temperature of charge rise to -15~-20 DEG C from -30~-35 DEG C in 100~200w in 4 hours；Adjust microwave generator
Microwave power to 200~300w, so that temperature of charge is risen to 0 DEG C from -15~-20 DEG C in 2 hours；Microwave generator is adjusted again
Microwave power to 300~400w, so that temperature of charge is risen to 30 DEG C from 0 DEG C in 1 hour, after bleeding off pressure from dryness storehouse take out, obtain
It is 5% freeze-drying prods below to biodiversity content.
Preferably, step 6) are as follows: by biodiversity content after vacuum freeze drying be 5% freeze-drying prods below, 30
DEG C or less carry out crushing 8min with airslide disintegrating mill so that 95% or more grain size of micropowder reaches 15 μm hereinafter, super up to ginseng fructus lycii
Micro mist.
Compared with prior art, the invention has the following beneficial technical effects.
The transform power microwave and vacuum freeze drying combination technology that the present invention uses, are integrally added using microwave drying medium
Heat, without the heat transfer of other heat transfer, when avoiding heat transmission resistance and the thermal losses of conductive process, therefore shortening freeze-drying
Between, reduce drying cost.To change, conventional vacuum freeze-drying existing drying time is long, energy consumption consumption is big, drying
Disadvantage at high cost also solves the distillation in conventional vacuum freeze-drying method using heating plate to fructus lycii, ginseng moisture and mentions
Supplying heat source makes the disadvantages of product uneven heating is even, surface mass is denaturalized, surface part color blacks.Dry each stage pair simultaneously
Energy requirement is different, and the present invention uses different capacity microwave, on the one hand reduces specific energy consumption, on the other hand solves part because of temperature
It spends high and generates the problems such as product colour turns yellow, is charred and glow discharge phenomenon.
Since the polyoses content inside fructus lycii is very high, using conventional vacuum freeze-drying method can exist drying time it is long,
The disadvantages of energy consumption consumption is big, drying cost is high, and the present inventor has found by many experiments, and fructus lycii, ginseng are carried out powder together
Broken processing, using in ginseng, there are more lignin, cellulose, starch, protein etc., can solve drying time length, energy
The problems such as consumption consumption is big, drying cost is high.
By being stirred to ginseng, fructus lycii concentrate with high-speed mixer, be passed through while stirring nitrogen or other
Inert gas is allowed to become porous material, and constructed pore structure forms effective moisture liter in later period drying process
Magnificent duct makes internal moisture improve using energy source to improve rates for freeze-drying by distillation duct rapid sublimation evolution
Rate achievees the purpose that rapid freeze-drying.Would not also be generated by dry material ice-melt, collapse, drying shrinkage, shrinkage, surface rise drum the problems such as,
Also it provides convenience to the crushing in later period.
By a series of combination of technologies, as long as so as to reach freezing dry process of the present invention 6~8 hours time-consuming, and it is general
The time-consuming of logical freeze-drying is 20~35 hours, all at least at least shortens one times than general freezer drying in terms of time and energy consumption
More than.
For the present invention by the operation such as reverse osmosis concentration, freeze-drying, low-temperature grinding, whole process is all in low temperature environment
It is handled, can avoid the effective component occurred oxidation, the quality deteriorations reaction such as volatile oil and other heat-sensitive substances are destroyed.
The reduction of chemical reaction velocity and the passivation of enzyme under cryogenic, so that almost without enzyme and amino acid in freezing dry process
Caused browning phenomenon, guarantee it is dry after appearance, color and fresh consistent, drug effect, quality do not change.Sufficiently keep
Fresh ginseng, the effective component of fructus lycii, nutritional ingredient, product rehydration obtained is high, its color after adding water to restore, quality with it is fresh
Product do not have difference substantially.
Ginseng wolfberry fruit powder obtained by drying process of the present invention had not only maintained the fine quality of conventional vacuum freeze-drying, but also shortened
Time of vacuum freeze-drying technique, reduce energy consumption.
The research of the invention finds that fresh ginseng, fructus lycii are lyophilized under the conditions of present invention process, can be effectively retained
Ginsenoside Rg1, ginsenoside Re, ginsenoside Rb1, polysaccharide, the active constituent contents such as glycine betaine, it is good to maintain product
Rehydration, while freeze-drying time is effectively saved, energy consumption of freeze drying is reduced, the saving of production cost is conducive to, has reached best
Freeze drying rate.
Product after present invention freeze-drying using vacuum or nitrogen-filled packaging and is kept in dark place, long shelf-life.Be more advantageous to ginseng,
The stability of fructus lycii during storage.
Specific embodiment
Below with reference to embodiment, the present invention is further explained, but is not intended to limit the scope of the invention.
Embodiment 1
A kind of ginseng fructus lycii Ultramicro-powder microwave vacuum freeze drying means, method includes the following steps:
1) it pre-processes: by the ginseng of fresh harvesting, fructus lycii, silt is eluted with water, drains；
2) it is beaten: being 1:1:2 by pretreated ginseng, fructus lycii and water proportions, be put into high-speed shearing machine and be beaten；
3) it is concentrated: the slurries of step 2 is turned through reverse osmosis unit, reverse osmotic pressure is 0.1~4.0MPa, controls reverse osmosis membrane filtration
Excess temperature is 0~30 DEG C, and running to the partial volume that shuts off is the 40% of total volume, takes out concentrate；
4) precooling: the concentrate that step 3) is concentrated through reverse osmosis unit -10~0 DEG C at a temperature of, use high-speed mixer
It is stirred, is passed through nitrogen while stirring, be allowed to become porous material, porosity to 50%；It is then pre- at -35 DEG C
Freeze 0.5 hour, guarantees that concentrate sufficiently freezes；
5) it is freeze-dried: the cold well temperature of dryness storehouse being first down to -35 DEG C hereinafter, being then put into step 4) Cryo-concentration liquid
In dryness storehouse, dryness storehouse is vacuumized, vacuum degree opens microwave generator control microwave power 100 after reaching 20~100Pa
~200w makes temperature of charge rise to -15~-20 DEG C from -30~-35 DEG C in 3 hours；Adjust the microwave power of microwave generator
To 200~300w, temperature of charge is made to rise to 0 DEG C from -15~-20 DEG C in 3 hours；The microwave power of microwave generator is adjusted again
To 300~400w, temperature of charge is made to rise to 30 DEG C from 0 DEG C in 2 hours, is taken out after bleeding off pressure from dryness storehouse, obtain biodiversity
Content is 5% freeze-drying prods below；
6) it crushes: being 5% freeze-drying prods below by biodiversity content after vacuum freeze drying, use air-flow powder at 30 DEG C or less
Broken machine carries out crushing 8min, so that 95% or more grain size of micropowder reaches 15 μm hereinafter, up to ginseng fructus lycii Ultramicro-powder；
7) it packs: ginseng fructus lycii Ultramicro-powder is fitted into clean packaging, airtight vacuum or rush nitrogen and pack.
Embodiment 2
A kind of ginseng fructus lycii Ultramicro-powder microwave vacuum freeze drying means, method includes the following steps:
1) it pre-processes: by the ginseng of fresh harvesting, fructus lycii, silt is eluted with water, drains；
2) it is beaten: being 1:0.5:4 by pretreated ginseng, fructus lycii and water proportions, be put into high-speed shearing machine and be beaten；
3) it is concentrated: the slurries of step 2 is turned through reverse osmosis unit, reverse osmotic pressure is 0.1~4.0MPa, controls reverse osmosis membrane filtration
Excess temperature is 0~30 DEG C, and running to the partial volume that shuts off is the 25% of total volume, takes out concentrate；
4) precooling: the concentrate that step 3) is concentrated through reverse osmosis unit -10~0 DEG C at a temperature of, use high-speed mixer
It is stirred, is passed through nitrogen while stirring, be allowed to become porous material, porosity to 30%；It is then pre- at -35 DEG C
Freeze 1 hour, guarantees that concentrate sufficiently freezes；
5) it is freeze-dried: the cold well temperature of dryness storehouse being first down to -35 DEG C hereinafter, being then put into step 4) Cryo-concentration liquid
In dryness storehouse, dryness storehouse is vacuumized, vacuum degree opens microwave generator control microwave power 100 after reaching 20~100Pa
~200w makes temperature of charge rise to -15~-20 DEG C from -30~-35 DEG C in 4 hours；Adjust the microwave power of microwave generator
To 200~300w, temperature of charge is made to rise to 0 DEG C from -15~-20 DEG C in 2 hours；The microwave power of microwave generator is adjusted again
To 300~400w, temperature of charge is made to rise to 30 DEG C from 0 DEG C in 1 hour, is taken out after bleeding off pressure from dryness storehouse, obtain biodiversity
Content is 5% freeze-drying prods below；
6) it crushes: being 5% freeze-drying prods below by biodiversity content after vacuum freeze drying, use air-flow powder at 30 DEG C or less
Broken machine carries out crushing 5min, so that 95% or more grain size of micropowder reaches 15 μm hereinafter, up to ginseng fructus lycii Ultramicro-powder；
7) it packs: ginseng fructus lycii Ultramicro-powder is fitted into clean packaging, airtight vacuum or rush nitrogen and pack.
Embodiment 3
A kind of ginseng fructus lycii Ultramicro-powder microwave vacuum freeze drying means, method includes the following steps:
1) it pre-processes: by the ginseng of fresh harvesting, fructus lycii, silt is eluted with water, drains；
2) it is beaten: being 1:2:10 by pretreated ginseng, fructus lycii and water proportions, be put into high-speed shearing machine and be beaten；
3) it is concentrated: the slurries of step 2 is turned through reverse osmosis unit, reverse osmotic pressure is 0.1~4.0MPa, controls reverse osmosis membrane filtration
Excess temperature is 0~30 DEG C, and running to the partial volume that shuts off is the 10% of total volume, takes out concentrate；
4) precooling: the concentrate that step 3) is concentrated through reverse osmosis unit -10~0 DEG C at a temperature of, use high-speed mixer
It is stirred, is passed through nitrogen while stirring, be allowed to become porous material, porosity to 20%；It is then pre- at -30 DEG C
Freeze 2 hours, guarantees that concentrate sufficiently freezes；
5) it is freeze-dried: the cold well temperature of dryness storehouse being first down to -35 DEG C hereinafter, being then put into step 4) Cryo-concentration liquid
In dryness storehouse, dryness storehouse is vacuumized, vacuum degree opens microwave generator control microwave power 100 after reaching 20~100Pa
~200w makes temperature of charge rise to -15~-20 DEG C from -30~-35 DEG C in 4 hours；Adjust the microwave power of microwave generator
To 200~300w, temperature of charge is made to rise to 0 DEG C from -15~-20 DEG C in 2 hours；The microwave power of microwave generator is adjusted again
To 300~400w, temperature of charge is made to rise to 30 DEG C from 0 DEG C in 2 hours, is taken out after bleeding off pressure from dryness storehouse, obtain biodiversity
Content is 5% freeze-drying prods below；
6) it crushes: being 5% freeze-drying prods below by biodiversity content after vacuum freeze drying, use air-flow powder at 30 DEG C or less
Broken machine carries out crushing 10min, so that 95% or more grain size of micropowder reaches 15 μm hereinafter, up to ginseng fructus lycii Ultramicro-powder；
7) it packs: ginseng fructus lycii Ultramicro-powder is fitted into clean packaging, airtight vacuum or rush nitrogen and pack.
Glycine betaine detection method in sample.
It takes this product to shred, takes about 2g, it is accurately weighed, add 80% methanol 50ml, be heated to reflux 1 hour, let cool, filter, uses
80% methanol 30ml washs residue and filter by several times, merges washing lotion and filtrate, is concentrated into 10ml, with salt acid for adjusting pH value to 1, adds
Entering active carbon 1g, heating is boiled, and is let cool, and is filtered, and it is washed by several times with water 15ml, merges washing lotion and filtrate, what addition was newly prepared
2.5% chromic thiocyanate ammonium salt solution 20ml, stirs evenly, and 10 DEG C 3 hours arranged below.It is filtered with G4 sintered filter funnel, precipitates a small amount of ice water
Washing, is drained, residue adds acetone solution, is transferred in 5ml measuring bottle, adds acetone to scale, shakes up, as test solution.
Separately take glycine betaine reference substance appropriate, it is accurately weighed, add methanol hydrochloride solution (0.5 → 100) that every 1ml is made containing 4mg
Solution, as reference substance solution.
It is tested according to thin-layered chromatography (general rule 0502), precision draws 5 μ l of test solution, reference substance solution 3 μ l and 6 μ l,
Crosspoint is on same silica gel g thin-layer plate respectively, and with acetone-dehydrated alcohol-hydrochloric acid (10:6:1) for solvent, presaturation 30 divides
Clock is unfolded, and takes out, volatilizes solvent, sprays the improvement bismuth potassium iodide test solution newly to prepare immediately, and placement 1~3 hour clear to spot
It is clear, it is scanned according to thin-layered chromatography (general rule 0502), wavelength: λ S=515nm, λ R=590nm, measurement test sample absorbance integral
Value with reference substance absorbance integrated value, calculate to get.
Ginsenoside Re's detection method in sample.
Chromatographic condition and system suitability: using octadecylsilane chemically bonded silica as filler；It is flowing with acetonitrile
Phase A, using water as Mobile phase B, the regulation according to the form below carries out gradient elution；Detection wavelength is 203nm.Number of theoretical plate presses ginseng soap
The peak glycosides Re, which calculates, should be not less than 6000.
| Time (minute) | Mobile phase A (%) | Mobile phase B (%) |
| 0~35 | 19 | 81 |
| 35~55 | 19→29 | 81→71 |
| 55~70 | 29 | 71 |
| 70~100 | 29→40 | 71→60 |
The preparation of reference substance solution: precision weighs ginsenoside Re's reference substance, adds methanol that every 1ml is made containing the molten of 0.2mg
Liquid, shake up to get.
The preparation of test solution: taking this product powder (crossing No. four sieves) about 1g, accurately weighed, sets in Soxhlet extractor, adds
Chloroform is heated to reflux 3 hours, discards chloroform liquid, and the dregs of a decoction volatilize solvent, moves into 100ml conical flask together with filtration paper cylinder
In, precision plus water-saturated n-butanol 50ml, close plug are stood overnight, ultrasonic treatment (power 250W, frequency 50kHz) 30 minutes, filter
It crosses, discards primary filtrate, precision measures subsequent filtrate 25ml, sets in evaporating dish and be evaporated, residue adds methanol to dissolve and is transferred to 5ml measuring bottle
In, add methanol dilution to shake up to scale, filter, take subsequent filtrate to get.
Measuring method: it is accurate respectively to draw 10 μ l of reference substance solution and 10~20 μ l of test solution, liquid chromatograph is injected,
Measurement to get.
Control group is set simultaneously, and control group is prepared using the furnace drying method of fresh ginseng, fructus lycii mixed serum and routine
Ultramicro-powder.
| Title | Appearance | Glycine betaine (%) (based on dry product) | Ginsenoside Re's (%) (based on dry product) |
| Embodiment 1 | Light red | 0.62 | 0.33 |
| The Ultramicro-powder of oven drying method preparation | Brownish red | 0.45 | 0.22 |
| Fresh ginseng, fructus lycii mixed serum | Light red | 0.64 | 0.36 |
Ginseng wolfberry fruit powder obtained by drying process of the present invention had not only maintained the fine quality of conventional vacuum freeze-drying, but also shortened
Time of vacuum freeze-drying technique, reduce energy consumption.
The research of the invention finds that fresh ginseng, fructus lycii are lyophilized under the conditions of present invention process, can be effectively retained
Ginsenoside Rg1, ginsenoside Re, ginsenoside Rb1, polysaccharide, the active constituent contents such as glycine betaine, it is good to maintain product
Rehydration, while freeze-drying time is effectively saved, energy consumption of freeze drying is reduced, the saving of production cost is conducive to, has reached best
Freeze drying rate.
Claims (4)
1. a kind of ginseng fructus lycii Ultramicro-powder microwave vacuum freeze drying means, it is characterised in that this method includes the following steps:
1) it pre-processes: by the ginseng of fresh harvesting, fructus lycii, silt is eluted with water, drains；
2) it is beaten: being 1:0.5~2:2~10 by pretreated ginseng, fructus lycii and water proportions, be put into high-speed shearing machine progress
Mashing；
3) it is concentrated: the slurries of step 2 is turned through reverse osmosis unit, reverse osmotic pressure is 0.1~4.0MPa, controls reverse osmosis membrane filtration
Excess temperature is 0~30 DEG C, and running to the partial volume that shuts off is the 10~40% of total volume, takes out concentrate；
4) precooling: the concentrate that step 3) is concentrated through reverse osmosis unit -10~0 DEG C at a temperature of, use high-speed mixer
It is stirred, is passed through gas while stirring, be allowed to become porous material；The then pre-freeze 0.5~2 at -30~-35 DEG C
Hour, guarantee that concentrate sufficiently freezes；
5) it is freeze-dried: the cold well temperature of dryness storehouse being first down to -35 DEG C hereinafter, being then put into step 4) Cryo-concentration liquid
In dryness storehouse, dryness storehouse is vacuumized, vacuum degree opens microwave generator control microwave power 100 after reaching 20~100Pa
~200w makes temperature of charge rise to -15~-20 DEG C from -30~-35 DEG C in 3~4 hours；Adjust the microwave of microwave generator
Power makes temperature of charge rise to 0 DEG C from -15~-20 DEG C to 200~300w in 2~3 hours；Microwave generator is adjusted again
Microwave power makes temperature of charge rise to 30 DEG C from 0 DEG C to 300~400w in 1~2 hour, takes out after bleeding off pressure from dryness storehouse,
Obtaining biodiversity content is 5% freeze-drying prods below；
6) it crushes: being 5% freeze-drying prods below by biodiversity content after vacuum freeze drying, use air-flow powder at 30 DEG C or less
Broken machine is crushed, so that 95% or more grain size of micropowder reaches 15 μm hereinafter, up to ginseng fructus lycii Ultramicro-powder；
7) it packs: ginseng fructus lycii Ultramicro-powder is fitted into clean packaging, airtight vacuum or rush nitrogen and pack.
2. the method according to claim 1, wherein the gas being passed through while stirring described in step 4) is nitrogen
Gas or other inert gases.
3. being allowed to the method according to claim 1, wherein being passed through gas while stirring described in step 4)
Become porous material, porosity to 20%~50%.
4. the method according to claim 1, wherein described in step 6) with airslide disintegrating mill carry out crushing 5~
10min。
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN112617149A (en) * | 2020-12-18 | 2021-04-09 | 湖北金贵中药饮片有限公司 | Preparation method of freeze-dried medlar |
| CN115153002A (en) * | 2022-07-13 | 2022-10-11 | 吉林农业大学 | Processing method of ginseng with complete shape |
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| CN106668321A (en) * | 2017-01-09 | 2017-05-17 | 宁夏早康生物科技有限公司 | Preparation method of radix ginseng and Chinese wolfberry fruit composition, and product and application thereof |
| CN107308350A (en) * | 2017-07-15 | 2017-11-03 | 浙江尖峰健康科技有限公司 | A kind of rhizoma Gastrodiae microwave vacuum freeze drying means |
| CN108669492A (en) * | 2018-05-17 | 2018-10-19 | 早康枸杞股份有限公司 | A kind of processing method and purposes of freeze-drying Wolfberry powder |
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Patent Citations (4)
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| CN102132879A (en) * | 2011-03-28 | 2011-07-27 | 韩红雯 | Process for freezing and drying medlar powder in vacuum |
| CN106668321A (en) * | 2017-01-09 | 2017-05-17 | 宁夏早康生物科技有限公司 | Preparation method of radix ginseng and Chinese wolfberry fruit composition, and product and application thereof |
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| CN108669492A (en) * | 2018-05-17 | 2018-10-19 | 早康枸杞股份有限公司 | A kind of processing method and purposes of freeze-drying Wolfberry powder |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN112617149A (en) * | 2020-12-18 | 2021-04-09 | 湖北金贵中药饮片有限公司 | Preparation method of freeze-dried medlar |
| CN115153002A (en) * | 2022-07-13 | 2022-10-11 | 吉林农业大学 | Processing method of ginseng with complete shape |
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