CN109432301A - A kind of dendrobium candidum ultrafine powder microwave vacuum freeze drying means - Google Patents
A kind of dendrobium candidum ultrafine powder microwave vacuum freeze drying means Download PDFInfo
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- CN109432301A CN109432301A CN201811310327.3A CN201811310327A CN109432301A CN 109432301 A CN109432301 A CN 109432301A CN 201811310327 A CN201811310327 A CN 201811310327A CN 109432301 A CN109432301 A CN 109432301A
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- F26B—DRYING SOLID MATERIALS OR OBJECTS BY REMOVING LIQUID THEREFROM
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- F26B5/04—Drying solid materials or objects by processes not involving the application of heat by evaporation or sublimation of moisture under reduced pressure, e.g. in a vacuum
- F26B5/048—Drying solid materials or objects by processes not involving the application of heat by evaporation or sublimation of moisture under reduced pressure, e.g. in a vacuum in combination with heat developed by electro-magnetic means, e.g. microwave energy
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Abstract
The invention discloses a kind of dendrobium candidum ultrafine powder microwave vacuum freeze drying means, include the following steps: 1) to pre-process: by the dendrobium candidum stem item of fresh harvesting, related blade, Hua Yiqi are eluted with water silt, drain；2) it is beaten: by pretreated dendrobium candidum, water mashing is added；3) it is concentrated: dendrobium candidum slurries is turned to be concentrated through reverse osmosis unit；4) precooling: the dendrobium candidum 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 dendrobium candidum ultrafine 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 dendrobium candidum more particularly to a kind of dendrobium candidum ultrafine powder microwave vacuum are cold
Drying method is lyophilized.
Background technique
Dendrobium candidum is the perennial herbaceous plant that grows nonparasitically upon another plant of orchid family.It is born in the height above sea level rock dark and damp up to 1600 meters of mountainous region half
On, the environment of warm and moist weather and half yin and half yang is liked, can not resist cold.Generally it is resistant to -5 DEG C of low temperature.Dendrobium nobile can be divided into Huang
Tens of kinds of grass, Jin Chai, horsewhip etc., dendrobium candidum is the superfine product of dendrobium nobile, it gains the name because epidermis is green in iron.Dendrobium candidum has
Unique medical value is used as medicine with its stem, belongs to the yin tonics in tonic, " Chinese Pharmacopoeia ": reinforcing stomach reg fluid, nourishing Yin and clearing heat.Iron
The tender stem of the minority kind such as skin dendrobium nobile, can also carry out special processing, be twisted into helical form or spring like, dry, commodity are known as ear
Ring dendrobium nobile also known as maple bucket.
Tang opens Taoist school between the first year classical " Taoist Scriptures " for dendrobium candidum, Herba Saussureae Involueratae, three double ginsengs, 120 years head
Crow, the Poria cocos of cycle of sixty years, desert cistanche, remote mountains ganoderma lucidum, seabed pearl, cordyceps sinensis etc. are classified as Chinese nine big " mesonas ".Over the past thousands of years, exist
South is civil, and when having urgent patient to be in critically ill, people can emit life danger from overhanging cliff by every means
It adopts and comes " mesona ", its juice is fed in disease population, patient is enabled to come back to life.Although this saying has its legendry, but according to
It carries, civil to be implicitly present in this medicinal material for being referred to as " help mesona ", its scientific name is called " dendrobium candidum ".
The application of dendrobium candidum, early in the Shennong's Herbal in Eastern Han Dynasty's last years of a dynasty or reign just on the books, Compendium of Material Medica, " Chinese medicine
Dictionary " etc. the medicinal function of dendrobium candidum is all described in Ancient Times in China multi-section medical literature." dendrobium candidum " is in Chinese medicine
Bed application has had thousands of years history, is known as the good reputation of enriching yin panacea.Dendrobium candidum is economical in Dendrobium Sw at this stage
Be worth highest type, purposes is mainly medicinal and health care product uses, dendrobium candidum pharmaceutically have promote the production of body fluid, quench the thirst, town
Bitterly, the effect of eliminating oedema, cures mainly that the pyreticosis deficiency of Yin, mesh are dark, stomach is weak, scorching, chronic branch is waited in the pharynx of hoarseness, diabetes, acute and chronic
The diseases such as tracheitis, tuberculosis, chronic liver disease, atrophic gastritis, immunologic hypofunction, burnout syndrome, tired to vocal cords,
Restore its U.S. sound to have specific characteristics curative effect, plants value with important exploitation.
Freeze Drying Technique is much studied and is reported in the application of the dry processing of dendrobium candidum at present, it with dry,
The dendrobium candidum of hot-air seasoning production is compared, not only polysaccharide, mannose, alkaloid, microelement, luxuriant and rich with fragrance class compound, bibenzyl
Class compound, alkane derivative and heat-sensitive ingredients etc. are not damaged, and can keep color, the battalion of fresh goods to the maximum extent
It forms point, appearance and active material.Such as: number of patent application: 201510154489.2, disclose fresh dendrobium candidum freeze-dried powder and
Preparation method, it is to take fresh orchid dendrobium candidum, adds water to remove impurity, cuts into segment；1/5~1/4 amount of dissection product is taken,
- 70 DEG C of freezer units are set to freeze 6~15 hours；Remaining dissection product are taken to set freeze drier, at -35 DEG C or less pre-freezes at least 2 hours,
Then 1/5~1/4 dissection product freezed in advance are incorporated to freeze drier, whole dissection product is mixed；Make in freeze drier
Dissection product carry out distillation parsing 15~30 hours so that dissection virtue moisture be down to 5% hereinafter, dissection lyophilized products；Take dissection
Lyophilized products are crushed with pulverizer, until powder size is less than 50 mesh to get fresh dendrobium candidum freeze-dried powder.Number of patent application:
201410426017.3, the dendrobium candidum of fresh harvesting is first cleaned, is drained, cut by dendrobium candidum freeze-dried powder and preparation method thereof
It is spare at the section of 2-4cm long；The dendrobium candidum section drained is placed in juice extractor, is added with the ratio of solid-liquid ratio 1g:5ml
Enter pure water to squeeze the juice；Dendrobium candidum juice is subjected to -20 DEG C of freeze overnights, it is spare；Vacuum freeze carries out again
The juice refrigerated product of dendrobium candidum are placed in the vacuum freeze by precooling treatment after -56 DEG C of pre-cooling half an hour, in
- 56 DEG C, carry out vacuum freeze drying under conditions of vacuum degree 7-9Pa and handle 18-30 hour, be lyophilized to obtain dendrobium candidum
Powder.Number of patent application: 201210569059.3, a kind of dendrobe ultrafine powder preparation process, sorting: taking dendrobium nobile, cuts into 1~2mm
Section；Grinding mashing: grinding after adding distilled water, and the additional amount of distilled water is 0.8~1.5 times of dendrobium nobile material quality；Pre-freeze: with
Being frozen into solid is standard, and maintains solid state 5~10 hours be frozen into, pre-freezing temperature -8~-18 DEG C；Freeze-drying: cold
It is the time 16~120 hours at -45~-50 DEG C that dry control condition, which is lyophilized,；It breaks micro mist: grinding is pulverized using oscillatory type
Kneading machine carries out the operation for being ground into micro mist so that 95% or more grain size of micropowder reach 10 μm hereinafter, dendrobe ultrafine powder moisture content
Lower than 5%.
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.Dendrobium candidum is squeezed the juice in certain methods or filters out juice after adding water mashing, just
It is freeze-dried by juice, is not accomplished full nutritional utilization dendrobium candidum effective component, cause dendrobium candidum utilization rate relatively low.
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 iron
The method of skin dendrobe ultrafine powder shortens the production cycle being entirely lyophilized, and specific energy consumption and cost, which is lyophilized, to be reduced, but also sufficiently
Effective component, the nutritional ingredient of fresh dendrobium candidum 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 dendrobium candidum ultrafine powder microwave vacuum freeze drying means, method includes the following steps:
1. a kind of dendrobium candidum ultrafine powder microwave vacuum freeze drying means, it is characterised in that this method includes the following steps:
1) pre-process: by the dendrobium candidum stem item of fresh harvesting, related blade, Hua Yiqi are eluted with water silt, drain；
2) it is beaten: by pretreated dendrobium candidum, 1~5 times of material quality of water mashing is added；
3) it is concentrated: the dendrobium candidum slurries of step 2 is turned through reverse osmosis unit, reverse osmotic pressure is 0.1~4.0MPa, and control is anti-
It is 0~30 DEG C that permeable membrane, which filters temperature, and running to the partial volume that shuts off is the 10~40% of total volume, takes out dendrobium candidum concentration
Liquid；
4) precooling: the dendrobium candidum concentrate that step 3) is concentrated through reverse osmosis unit -10~0 DEG C at a temperature of, with height
Fast blender is stirred, and is passed through gas while stirring, and is allowed to become porous material；It is then pre- at -30~-40 DEG C
Freeze 0.5~2 hour, guarantees that concentrate sufficiently freezes；
5) it is freeze-dried: the cold well temperature of dryness storehouse being first down to -40 DEG C hereinafter, being then put into step 4) Cryo-concentration liquid
In dryness storehouse, dryness storehouse is vacuumized, vacuum degree reach open after 10~50Pa microwave generator control microwave power 100~
200w makes temperature of charge rise to -20~-25 DEG C from -30~-40 DEG C in 3~4 hours；Adjust the microwave function of microwave generator
Rate makes temperature of charge rise to 0 DEG C from -20~-25 DEG C to 200~300w in 2~3 hours；The micro- of microwave generator is adjusted again
Wave power makes temperature of charge rise to 30 DEG C from 0 DEG C to 300~400w in 1~2 hour, takes out, obtains from dryness storehouse after bleeding off pressure
It is 5% freeze-drying dendrobium candidum below to biodiversity content；
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 dendrobium candidum ultrafine powder；
7) it packs: dendrobium candidum ultrafine powder is fitted into clean packaging, airtight vacuum or rush nitrogen and pack.
Preferably, step 4) are as follows: the dendrobium candidum concentrate that step 3) is concentrated through reverse osmosis unit is at -10~0 DEG C
At a temperature of, it is stirred with high-speed mixer, is passed through nitrogen while stirring, be allowed to become porous material, porosity is extremely
25%；Then pre-freeze 1 hour at -30~-40 DEG C guarantees that concentrate sufficiently freezes.
Preferably, step 5) are as follows: the cold well temperature of dryness storehouse is first down to -40 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 10~50Pa
Power makes temperature of charge rise to -20~-25 DEG C from -30~-40 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 -20~-25 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 dendrobium candidum 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 dendrobium candidum
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 dendrobium candidum moisture and provides
Heat source makes the disadvantages of dendrobium candidum uneven heating is even, surface mass is denaturalized, surface part color blacks.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 colloid, the mucus juice content inside dendrobium candidum stem item are very high, using conventional vacuum freeze-drying method meeting
The disadvantages of there are drying time is long, energy consumption consumption is big, drying cost is high, and the present inventor has found by many experiments, by iron sheet
The related blade of stem of Dendrobium item, flower carry out crushing and processing together, using dendrobium candidum leaf, spend that middle there are more lignin, fiber
Element, starch, protein etc. can solve the problems such as drying time is long, energy consumption consumption is big, drying cost is high, also solved fresh
Dendrobium candidum and conventional dried frozen aquatic products chew the problems such as glutinous mouth, glutinous tooth.
By being stirred to dendrobium candidum concentrate with high-speed mixer, it is passed through nitrogen while stirring or other are lazy
Property gas, is allowed to become porous material, constructed pore structure forms effective water sublimed in later period drying process
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 15~30 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 guarantees that the appearance after dendrobium candidum is dry, color are consistent with fresh dendrobium candidum, and drug effect, quality are not
It changes.Effective component, the nutritional ingredient of fresh dendrobium candidum are sufficiently kept, product rehydration obtained is high, and water is added to restore
Its color, quality and fresh goods there are not difference substantially afterwards.
Dendrobium candidum obtained by drying process of the present invention had both maintained the fine quality of conventional vacuum freeze-drying dendrobium candidum,
The time for shortening vacuum freeze-drying technique again, reduce energy consumption.
The research of the invention finds that fresh dendrobium candidum is lyophilized under the conditions of present invention process, can be effectively retained
The active constituent contents such as polysaccharide, mannose, dendrobine, maintain the good rehydration of product, while when effectively saving freeze-drying
Between, energy consumption of freeze drying is reduced, the saving of production cost is conducive to, has reached optimal 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 iron sheet
The stability of dendrobium nobile 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 dendrobium candidum ultrafine powder microwave vacuum freeze drying means, method includes the following steps:
1) pre-process: by the dendrobium candidum stem item of fresh harvesting, related blade, Hua Yiqi are eluted with water silt, drain；
2) it is beaten: by pretreated dendrobium candidum, 1 times of material quality of water mashing is added；
3) it is concentrated: the dendrobium candidum slurries of step 2 is turned through reverse osmosis unit, reverse osmotic pressure is 0.1~4.0MPa, and control is anti-
It is 0~30 DEG C that permeable membrane, which filters temperature, and running to the partial volume that shuts off is the 40% of total volume, takes out dendrobium candidum concentrate；
4) precooling: the dendrobium candidum concentrate that step 3) is concentrated through reverse osmosis unit -10~0 DEG C at a temperature of, with height
Fast blender is stirred, and is passed through nitrogen while stirring, and is allowed to become porous material, porosity to 50%；Then-
Pre-freeze 0.5 hour at 40 DEG C guarantees that concentrate sufficiently freezes；
5) it is freeze-dried: the cold well temperature of dryness storehouse being first down to -40 DEG C hereinafter, being then put into step 4) Cryo-concentration liquid
In dryness storehouse, dryness storehouse is vacuumized, vacuum degree reach open after 10~50Pa microwave generator control microwave power 100~
200w makes temperature of charge rise to -20~-25 DEG C from -30~-40 DEG C in 3 hours；The microwave power of adjustment microwave generator arrives
200~300w makes temperature of charge rise to 0 DEG C from -20~-25 DEG C in 3 hours；The microwave power for adjusting microwave generator again arrives
300~400w makes temperature of charge rise to 30 DEG C from 0 DEG C in 2 hours, takes out after bleeding off pressure from dryness storehouse, obtains biodiversity and contain
Amount is 5% freeze-drying dendrobium candidum 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 dendrobium candidum ultrafine powder；
7) it packs: dendrobium candidum ultrafine powder is fitted into clean packaging, airtight vacuum or rush nitrogen and pack.
Embodiment 2
A kind of dendrobium candidum ultrafine powder microwave vacuum freeze drying means, method includes the following steps:
1) pre-process: by the dendrobium candidum stem item of fresh harvesting, related blade, Hua Yiqi are eluted with water silt, drain；
2) it is beaten: by pretreated dendrobium candidum, 3 times of material quality of water mashing is added；
3) it is concentrated: the dendrobium candidum slurries of step 2 is turned through reverse osmosis unit, reverse osmotic pressure is 0.1~4.0MPa, and control is anti-
It is 0~30 DEG C that permeable membrane, which filters temperature, and running to the partial volume that shuts off is the 25% of total volume, takes out dendrobium candidum concentrate；
4) precooling: the dendrobium candidum concentrate that step 3) is concentrated through reverse osmosis unit -10~0 DEG C at a temperature of, with height
Fast blender is stirred, and is passed through nitrogen while stirring, and is allowed to become porous material, porosity to 30%；Then-
Pre-freeze 1 hour at 35 DEG C guarantees that concentrate sufficiently freezes；
5) it is freeze-dried: the cold well temperature of dryness storehouse being first down to -40 DEG C hereinafter, being then put into step 4) Cryo-concentration liquid
In dryness storehouse, dryness storehouse is vacuumized, vacuum degree reach open after 10~50Pa microwave generator control microwave power 100~
200w makes temperature of charge rise to -20~-25 DEG C from -30~-40 DEG C in 4 hours；The microwave power of adjustment microwave generator arrives
200~300w makes temperature of charge rise to 0 DEG C from -20~-25 DEG C in 2 hours；The microwave power for adjusting microwave generator again arrives
300~400w makes temperature of charge rise to 30 DEG C from 0 DEG C in 1 hour, takes out after bleeding off pressure from dryness storehouse, obtains biodiversity and contain
Amount is 5% freeze-drying dendrobium candidum 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 dendrobium candidum ultrafine powder；
7) it packs: dendrobium candidum ultrafine powder is fitted into clean packaging, airtight vacuum or rush nitrogen and pack.
Embodiment 3
A kind of dendrobium candidum ultrafine powder microwave vacuum freeze drying means, method includes the following steps:
1) pre-process: by the dendrobium candidum stem item of fresh harvesting, related blade, Hua Yiqi are eluted with water silt, drain；
2) it is beaten: by pretreated dendrobium candidum, 5 times of material quality of water mashing is added；
3) it is concentrated: the dendrobium candidum slurries of step 2 is turned through reverse osmosis unit, reverse osmotic pressure is 0.1~4.0MPa, and control is anti-
It is 0~30 DEG C that permeable membrane, which filters temperature, and running to the partial volume that shuts off is the 10% of total volume, takes out dendrobium candidum concentrate；
4) precooling: the dendrobium candidum concentrate that step 3) is concentrated through reverse osmosis unit -10~0 DEG C at a temperature of, with height
Fast blender is stirred, and is passed through nitrogen while stirring, and is allowed to become porous material, porosity to 20%；Then-
Pre-freeze 2 hours at 30 DEG C guarantee that concentrate sufficiently freezes；
5) it is freeze-dried: the cold well temperature of dryness storehouse being first down to -40 DEG C hereinafter, being then put into step 4) Cryo-concentration liquid
In dryness storehouse, dryness storehouse is vacuumized, vacuum degree reach open after 10~50Pa microwave generator control microwave power 100~
200w makes temperature of charge rise to -20~-25 DEG C from -30~-40 DEG C in 4 hours；The microwave power of adjustment microwave generator arrives
200~300w makes temperature of charge rise to 0 DEG C from -20~-25 DEG C in 2 hours；The microwave power for adjusting microwave generator again arrives
300~400w makes temperature of charge rise to 30 DEG C from 0 DEG C in 2 hours, takes out after bleeding off pressure from dryness storehouse, obtains biodiversity and contain
Amount is 5% freeze-drying dendrobium candidum 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 dendrobium candidum ultrafine powder；
7) it packs: dendrobium candidum ultrafine powder is fitted into clean packaging, airtight vacuum or rush nitrogen and pack.
Polysaccharide detection method in sample.
The preparation of reference substance solution: taking DEXTROSE ANHYDROUS reference substance appropriate, accurately weighed, adds water that every 1ml is made containing 90 μ g
Solution to get.The preparation precision of standard curve measures reference substance solution 0.2ml, 0.4ml, 0.6ml, 0.8ml, 1.0ml, point
Do not set in 10ml tool plug test tube, respectively plus water is mended to 1.0ml, and precision is added 5% phenol solution 1ml(and faces with preparation), it shakes up, then essence
Close plus sulfuric acid 5ml, shakes up, sets in boiling water bath and heat 20 minutes, takes out, and sets cooling 5 minutes in ice bath, is sky with corresponding reagent
It is white, according to UV-VIS spectrophotometry, absorbance is measured at the wavelength of 488nm, using absorbance as ordinate, concentration is cross
Coordinate draws standard curve.
The preparation of test solution: taking this product powder (crossing No. three sieves) about 0.3g, accurately weighed, adds water 200ml, heats back
Stream 2 hours, lets cool, is transferred in 250ml measuring bottle, and with a small amount of moisture time washing container, washing lotion simultaneously in the same measuring bottle of people, is added water to
Scale shakes up, and filtration, precision measures subsequent filtrate 2ml, sets in 15ml centrifuge tube, and dehydrated alcohol 10ml is added in precision, shakes up, cold
1 hour, hiding is taken out, and centrifugation (revolving speed is 4000 turns per minute) 20 minutes discards supernatant liquid (filtering when necessary), precipitating plus 80%
Ethanol washing 2 times, each 8ml, centrifugation discards supernatant liquid, precipitating plus hot water dissolving, is transferred in 25ml measuring bottle, lets cool, add water
To scale, shake up to get.
Measuring method: precision measures test solution 1ml, sets in 10ml tool plug test tube, the side under sighting target directrix curve preparation
Method rises from " precision be added 5% phenol solution 1ml ", measures absorbance in accordance with the law, from nothing in reading test solution on standard curve
The amount of water glucose, calculate to get.
Mannose detection method in sample.
Chromatographic condition and system suitability are using octadecylsilane chemically bonded silica as filler；With acetonitrile-
The ammonium acetate solution (20:80) of 0.02mol/L is mobile phase；Detection wavelength is 250nm.Number of theoretical plate is answered by the calculating of mannose peak
Not less than 4000.
Correction factor measurement: taking aminoglucose hydrochloride appropriate, accurately weighed, adds water that solution of every 1ml containing 12mg is made,
As inner mark solution.Mannose reference substance about 10mg separately is taken, it is accurately weighed, it sets in 100ml measuring bottle, inner mark solution is added in precision
1ml adds appropriate amount of water to make to dissolve and be diluted to scale, shakes up, and draws 400 μ l, adds the PMP(1- phenyl -3- methyl-of 0.5mol/L
5- pyrazolone) methanol solution and 0.3mol/L each 400 μ l of sodium hydroxide solution, mix, 70 DEG C water-bath 100 minutes.
Again plus the 500 μ l of hydrochloric acid solution of 0.3mol/L, mixing are washed 3 times, each 2ml discards chloroform liquid, water with chloroform
After the leafing heart, 10 μ l of supernatant is taken, injects liquid chromatograph, measurement calculates correction factor.
Measuring method: taking this product powder (crossing No. three sieves) about 0.12g, accurately weighed, sets in Soxhlet extractor, adds 80% ethyl alcohol
In right amount, heating and refluxing extraction 4 hours discard ethanol, and the dregs of a decoction volatilize ethyl alcohol, and filtration paper cylinder, which is dismantled, to be placed in a beaker, and add water
100ml, then accurate addition inner mark solution 2ml, decoct 1 hour and constantly stir, let cool, add water to mend to about 100ml, mix, from
The heart, Aspirate supernatant 1ml are set in ampoule bottle or ml headspace bottle, add the hydrochloric acid solution 0.5ml of 3.0mol/L, are sealed, and are mixed, 110 DEG C
Hydrolysis 1 hour, lets cool, and adjusts pH value to neutrality with the sodium hydroxide solution of 3.0mol/L, draws 400 μ l, survey according to correction factor
Determine method, from " the PMP methanol solution for adding 0.5mol/L ", operate according to methods, supernatant is taken to inject liquid chromatograph, measures, i.e.,
?.
Control group, the ultra micro that control group is prepared using fresh dendrobium candidum slurries and conventional furnace drying method are set simultaneously
Powder.
| Title | Appearance | Polysaccharide (%) (based on dry product) | Mannose (%) (based on dry product) |
| Embodiment 1 | Light green color | 27.1 | 24.1 |
| The Ultramicro-powder of oven drying method preparation | It is faint yellow | 22.8 | 20.5 |
| Fresh dendrobium candidum slurries | Light green color | 27.5 | 24.7 |
Dendrobium candidum obtained by drying process of the present invention had both maintained the fine quality of conventional vacuum freeze-drying dendrobium candidum,
The time for shortening vacuum freeze-drying technique again, reduce energy consumption.
The research of the invention finds that fresh dendrobium candidum is lyophilized under the conditions of present invention process, can be effectively retained
The active constituent contents such as polysaccharide, mannose, dendrobine, maintain the good rehydration of product, while when effectively saving freeze-drying
Between, energy consumption of freeze drying is reduced, the saving of production cost is conducive to, has reached optimal freeze drying rate.
Claims (4)
1. a kind of dendrobium candidum ultrafine powder microwave vacuum freeze drying means, it is characterised in that this method includes the following steps:
1) pre-process: by the dendrobium candidum stem item of fresh harvesting, related blade, Hua Yiqi are eluted with water silt, drain；
2) it is beaten: by pretreated dendrobium candidum, 1~5 times of material quality of water mashing is added；
3) it is concentrated: the dendrobium candidum slurries of step 2 is turned through reverse osmosis unit, reverse osmotic pressure is 0.1~4.0MPa, and control is anti-
It is 0~30 DEG C that permeable membrane, which filters temperature, and running to the partial volume that shuts off is the 10~40% of total volume, takes out dendrobium candidum concentration
Liquid；
4) precooling: the dendrobium candidum concentrate that step 3) is concentrated through reverse osmosis unit -10~0 DEG C at a temperature of, with height
Fast blender is stirred, and is passed through gas while stirring, and is allowed to become porous material；It is then pre- at -30~-40 DEG C
Freeze 0.5~2 hour, guarantees that concentrate sufficiently freezes；
5) it is freeze-dried: the cold well temperature of dryness storehouse being first down to -40 DEG C hereinafter, being then put into step 4) Cryo-concentration liquid
In dryness storehouse, dryness storehouse is vacuumized, vacuum degree reach open after 10~50Pa microwave generator control microwave power 100~
200w makes temperature of charge rise to -20~-25 DEG C from -30~-40 DEG C in 3~4 hours；Adjust the microwave function of microwave generator
Rate makes temperature of charge rise to 0 DEG C from -20~-25 DEG C to 200~300w in 2~3 hours；The micro- of microwave generator is adjusted again
Wave power makes temperature of charge rise to 30 DEG C from 0 DEG C to 300~400w in 1~2 hour, takes out, obtains from dryness storehouse after bleeding off pressure
It is 5% freeze-drying dendrobium candidum below to biodiversity content；
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 dendrobium candidum ultrafine powder；
7) it packs: dendrobium candidum ultrafine 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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| CN114304335A (en) * | 2021-12-21 | 2022-04-12 | 昆明生物制造研究院有限公司 | Method for enriching active ingredients of dendrobium leaves through fermentation and application of method |
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