CN109170869A - A kind of American ginseng medlar Ultramicro-powder microwave vacuum freeze drying means - Google Patents

A kind of American ginseng medlar Ultramicro-powder microwave vacuum freeze drying means Download PDF

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CN109170869A
CN109170869A CN201811310326.9A CN201811310326A CN109170869A CN 109170869 A CN109170869 A CN 109170869A CN 201811310326 A CN201811310326 A CN 201811310326A CN 109170869 A CN109170869 A CN 109170869A
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american ginseng
freeze
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powder
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胡爱娣
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    • A—HUMAN NECESSITIES
    • A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23L—FOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
    • A23L33/00—Modifying nutritive qualities of foods; Dietetic products; Preparation or treatment thereof
    • A—HUMAN NECESSITIES
    • A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23L—FOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
    • A23L3/00—Preservation of foods or foodstuffs, in general, e.g. pasteurising, sterilising, specially adapted for foods or foodstuffs
    • A23L3/34—Preservation of foods or foodstuffs, in general, e.g. pasteurising, sterilising, specially adapted for foods or foodstuffs by treatment with chemicals
    • A23L3/3409—Preservation of foods or foodstuffs, in general, e.g. pasteurising, sterilising, specially adapted for foods or foodstuffs by treatment with chemicals in the form of gases, e.g. fumigation; Compositions or apparatus therefor
    • A—HUMAN NECESSITIES
    • A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23L—FOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
    • A23L3/00—Preservation of foods or foodstuffs, in general, e.g. pasteurising, sterilising, specially adapted for foods or foodstuffs
    • A23L3/34—Preservation of foods or foodstuffs, in general, e.g. pasteurising, sterilising, specially adapted for foods or foodstuffs by treatment with chemicals
    • A23L3/3409—Preservation of foods or foodstuffs, in general, e.g. pasteurising, sterilising, specially adapted for foods or foodstuffs by treatment with chemicals in the form of gases, e.g. fumigation; Compositions or apparatus therefor
    • A23L3/3418—Preservation of foods or foodstuffs, in general, e.g. pasteurising, sterilising, specially adapted for foods or foodstuffs by treatment with chemicals in the form of gases, e.g. fumigation; Compositions or apparatus therefor in a controlled atmosphere, e.g. partial vacuum, comprising only CO2, N2, O2 or H2O
    • A—HUMAN NECESSITIES
    • A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23L—FOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
    • A23L3/00—Preservation of foods or foodstuffs, in general, e.g. pasteurising, sterilising, specially adapted for foods or foodstuffs
    • A23L3/40—Preservation of foods or foodstuffs, in general, e.g. pasteurising, sterilising, specially adapted for foods or foodstuffs by drying or kilning; Subsequent reconstitution
    • A23L3/44—Freeze-drying
    • A—HUMAN NECESSITIES
    • A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23L—FOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
    • A23L3/00—Preservation of foods or foodstuffs, in general, e.g. pasteurising, sterilising, specially adapted for foods or foodstuffs
    • A23L3/40—Preservation of foods or foodstuffs, in general, e.g. pasteurising, sterilising, specially adapted for foods or foodstuffs by drying or kilning; Subsequent reconstitution
    • A23L3/54—Preservation of foods or foodstuffs, in general, e.g. pasteurising, sterilising, specially adapted for foods or foodstuffs by drying or kilning; Subsequent reconstitution using irradiation or electrical treatment, e.g. ultrasonic waves
    • A—HUMAN NECESSITIES
    • A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23P—SHAPING OR WORKING OF FOODSTUFFS, NOT FULLY COVERED BY A SINGLE OTHER SUBCLASS
    • A23P10/00—Shaping or working of foodstuffs characterised by the products
    • A23P10/40—Shaping or working of foodstuffs characterised by the products free-flowing powder or instant powder, i.e. powder which is reconstituted rapidly when liquid is added
    • A—HUMAN NECESSITIES
    • A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23V—INDEXING SCHEME RELATING TO FOODS, FOODSTUFFS OR NON-ALCOHOLIC BEVERAGES AND LACTIC OR PROPIONIC ACID BACTERIA USED IN FOODSTUFFS OR FOOD PREPARATION
    • A23V2002/00—Food compositions, function of food ingredients or processes for food or foodstuffs

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  • Medicines Containing Plant Substances (AREA)

Abstract

The invention discloses a kind of American ginseng medlar Ultramicro-powder microwave vacuum freeze drying means, includes the following steps: 1) to pre-process: by the American Ginseng of fresh harvesting, fructus lycii, silt is eluted with water, drains；2) it is beaten: pretreated American 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 American Ginseng Ultramicro-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

A kind of American ginseng medlar Ultramicro-powder microwave vacuum freeze drying means
Technical field
The present invention relates to a kind of drying means of American ginseng medlar more particularly to a kind of American ginseng medlar Ultramicro-powder microwave are true Vacuum freecing-dry method.
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.
American Ginseng is Araliaceae Panax herbs perennial vegetation, alias American ginseng, American ginseng, Western ginseng, American Ginseng, originates in the Wisconsin State of Canadian big Quebec and the U.S., and the ground such as BeiJing, China Huairou and Changbai Mountain also have Plantation.American Ginseng is cool in nature, sweet in flavor, and slight bitter has the effects of boosting qi and nourishing yin, clearing heat and promoting fluid, is used for deficiency of vital energy yin deficiency, and abnormal heat is tired of tired, cough Breathe heavily phlegm blood, Heat Diabetes, dryness of the mouth and throat.Fructus lycii is mild-natured, sweet in flavor, returns liver and kidney channel, has nourishing liver and kidney, and benefiting shrewd head effect is used for Consumption consumptive loss, soreness of waist and knee joint, dizziness and tinnitus, impotence and seminal emission, Heat Diabetes, blood deficiency chlorosis, blurred vision.The two shares existing benefit Gas effect has nourishing yin effect again, and will not get angry after taking.
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 west The method of Sang-wolfberry-fruit Ultramicro-powder shortens the production cycle being entirely lyophilized, and specific energy consumption and cost, which is lyophilized, to be reduced, but also is filled Point new fresh fructus lycii, the effective component of American Ginseng, nutritional ingredient being kept, product rehydration obtained is high, its color after adding water to restore, Quality and fresh goods there are not difference substantially.
To achieve the goals above, present invention employs technique below and steps:
A kind of American ginseng medlar Ultramicro-powder microwave vacuum freeze drying means, method includes the following steps:
1. a kind of American ginseng medlar Ultramicro-powder microwave vacuum freeze drying means, it is characterised in that this method includes step below It is rapid:
1) it pre-processes: by the American Ginseng of fresh harvesting, fructus lycii, silt is eluted with water, drains；
2) be beaten: by pretreated American Ginseng, fructus lycii and water proportions be 1:0.5~2:2~10, be put into high-speed shearing machine into Row 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 American ginseng medlar Ultramicro-powder；
7) it packs: American ginseng medlar 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, up to American ginseng medlar Ultramicro-powder.
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 in conventional vacuum freeze-drying method using heating plate to fructus lycii, the distillation of American Ginseng moisture The disadvantages of heat source is provided, even product uneven heating, surface mass denaturation, surface part color is made to black.Dry each stage simultaneously To energy requirement difference, the present invention uses different capacity microwave, on the one hand reduces specific energy consumption, on the other hand solve part because Temperature is excessively 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, American Ginseng are carried out together Crushing and processing, using, there are more lignin, cellulose, starch, protein etc., having can solve drying time in American Ginseng The problems such as long, energy consumption consumption is greatly, drying cost is high.
By being stirred to American Ginseng, fructus lycii concentrate with high-speed mixer, be passed through while stirring nitrogen or its His inert gas, is allowed to become porous material, constructed pore structure forms effective moisture in later period drying process Distil duct, makes internal moisture by distillation duct rapid sublimation evolution, to improve rates for freeze-drying, improves energy benefit With rate, achieve the purpose that rapid freeze-drying.Would not also be generated by dry material ice-melt, collapse, drying shrinkage, shrinkage, surface rise drum etc. ask Topic, also 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 American Ginseng, the effective component of fructus lycii, nutritional ingredient, product rehydration obtained is high, its color after adding water to restore, quality with Fresh goods there is not difference substantially.
American ginseng medlar powder obtained by drying process of the present invention had not only maintained the fine quality of conventional vacuum freeze-drying, but also contracting The short time of vacuum freeze-drying technique, reduce energy consumption.
The research of the invention finds that fresh American Ginseng, fructus lycii are lyophilized under the conditions of present invention process, can effectively protect Stay ginsenoside Rg1, ginsenoside Re, ginsenoside Rb1, polysaccharide, the active constituent contents such as glycine betaine, it is good to maintain product Rehydration, while effectively saving freeze-drying time, reduce energy consumption of freeze drying, be conducive to the saving of production cost, reached most Good freeze drying rate.
Product after present invention freeze-drying using vacuum or nitrogen-filled packaging and is kept in dark place, long shelf-life.It is more advantageous to the West 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 American ginseng medlar Ultramicro-powder microwave vacuum freeze drying means, method includes the following steps:
1) it pre-processes: by the American Ginseng of fresh harvesting, fructus lycii, silt is eluted with water, drains；
2) it is beaten: being 1:1:2 by pretreated American 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 American ginseng medlar Ultramicro-powder；
7) it packs: American ginseng medlar Ultramicro-powder is fitted into clean packaging, airtight vacuum or rush nitrogen and pack.
Embodiment 2
A kind of American ginseng medlar Ultramicro-powder microwave vacuum freeze drying means, method includes the following steps:
1) it pre-processes: by the American Ginseng of fresh harvesting, fructus lycii, silt is eluted with water, drains；
2) it is beaten: being 1:0.5:4 by pretreated American 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 American ginseng medlar Ultramicro-powder；
7) it packs: American ginseng medlar Ultramicro-powder is fitted into clean packaging, airtight vacuum or rush nitrogen and pack.
Embodiment 3
A kind of American ginseng medlar Ultramicro-powder microwave vacuum freeze drying means, method includes the following steps:
1) it pre-processes: by the American Ginseng of fresh harvesting, fructus lycii, silt is eluted with water, drains；
2) it is beaten: being 1:2:10 by pretreated American 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 American ginseng medlar Ultramicro-powder；
7) it packs: American ginseng medlar 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 0.1% phosphoric acid solution as Mobile phase B, the regulation according to the form below carries out gradient elution；Detection wavelength is 203nm；Column temperature 40 ℃.Number of theoretical plate is calculated by ginsenoside Re peak should be not less than 5000.
Time (minute) Mobile phase A (%) Mobile phase B (%)
0~25 19→20 81→80
25~60 20→40 80→60
60~90 40→55 60→45
90~100 55→60 45→40
The preparation of reference substance solution: taking ginsenoside Re's reference substance appropriate, accurately weighed, adds methanol that every 1ml is made containing people Join saponin(e Re0.4mg solution to get.
The preparation of test solution: taking this product powder (crossing No. three sieves) about 1g, accurately weighed, sets in stuffed conical flask, essence Close that water saturated n-butanol 50ml is added, weighed weight is set heating and refluxing extraction 1.5 hours in water-bath, is let cool, then weighed heavy Amount, is saturated with water the weight that n-butanol supplies less loss, shakes up, and filters.Precision measures subsequent filtrate 25ml, sets in evaporating dish, is evaporated, Residue adds 50% methanol to make to dissolve in right amount, is transferred in 10ml measuring bottle, and 50% methanol is added to shake up to scale, filters, takes subsequent filtrate, To obtain the final product.
Measuring method: accurate absorption reference substance solution and each 10 μ l of test solution respectively, injection liquid chromatograph, measurement, To obtain the final product.
Control group is set simultaneously, and control group is prepared using the furnace drying method of fresh American 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 American Ginseng, fructus lycii mixed serum Light red 0.64 0.36
American ginseng medlar powder obtained by drying process of the present invention had not only maintained the fine quality of conventional vacuum freeze-drying, but also contracting The short time of vacuum freeze-drying technique, reduce energy consumption.
The research of the invention finds that fresh American Ginseng, fructus lycii are lyophilized under the conditions of present invention process, can effectively protect Stay ginsenoside Rg1, ginsenoside Re, ginsenoside Rb1, polysaccharide, the active constituent contents such as glycine betaine, it is good to maintain product Rehydration, while effectively saving freeze-drying time, reduce energy consumption of freeze drying, be conducive to the saving of production cost, reached most Good freeze drying rate.

Claims (4)

1. a kind of American ginseng medlar Ultramicro-powder microwave vacuum freeze drying means, it is characterised in that this method includes step below It is rapid:
1) it pre-processes: by the American Ginseng of fresh harvesting, fructus lycii, silt is eluted with water, drains；
2) be beaten: by pretreated American Ginseng, fructus lycii and water proportions be 1:0.5~2:2~10, be put into high-speed shearing machine into Row 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 American ginseng medlar Ultramicro-powder；
7) it packs: American ginseng medlar 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。
CN201811310326.9A 2018-11-06 2018-11-06 A kind of American ginseng medlar Ultramicro-powder microwave vacuum freeze drying means Withdrawn CN109170869A (en)

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Application publication date: 20190111