CN106344624A - Freeze-drying method for cordyceps sinensis - Google Patents
Freeze-drying method for cordyceps sinensis Download PDFInfo
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- 238000000034 method Methods 0.000 title claims abstract description 55
- 238000004108 freeze drying Methods 0.000 title claims abstract description 31
- 241001248610 Ophiocordyceps sinensis Species 0.000 title abstract description 9
- 238000001035 drying Methods 0.000 claims abstract description 23
- 238000000859 sublimation Methods 0.000 claims abstract description 16
- 230000008022 sublimation Effects 0.000 claims abstract description 16
- 238000001816 cooling Methods 0.000 claims abstract description 14
- 238000004140 cleaning Methods 0.000 claims abstract description 8
- 241000190633 Cordyceps Species 0.000 claims description 94
- 230000004087 circulation Effects 0.000 claims description 41
- 238000001179 sorption measurement Methods 0.000 claims description 16
- 230000011218 segmentation Effects 0.000 claims description 15
- 230000033228 biological regulation Effects 0.000 claims description 14
- 210000003746 feather Anatomy 0.000 claims description 11
- 230000008569 process Effects 0.000 claims description 10
- 238000003306 harvesting Methods 0.000 claims description 5
- FFRBMBIXVSCUFS-UHFFFAOYSA-N 2,4-dinitro-1-naphthol Chemical compound C1=CC=C2C(O)=C([N+]([O-])=O)C=C([N+]([O-])=O)C2=C1 FFRBMBIXVSCUFS-UHFFFAOYSA-N 0.000 abstract description 6
- 230000000694 effects Effects 0.000 abstract description 5
- 235000016709 nutrition Nutrition 0.000 abstract description 4
- 238000007710 freezing Methods 0.000 abstract description 2
- 230000008014 freezing Effects 0.000 abstract description 2
- 239000004615 ingredient Substances 0.000 abstract 1
- 235000019553 satiation Nutrition 0.000 abstract 1
- 239000002932 luster Substances 0.000 description 6
- 238000005516 engineering process Methods 0.000 description 5
- 230000035764 nutrition Effects 0.000 description 3
- 244000292693 Poa annua Species 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 201000010099 disease Diseases 0.000 description 2
- 208000037265 diseases, disorders, signs and symptoms Diseases 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 230000002085 persistent effect Effects 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- 244000283482 Alloteropsis cimicina Species 0.000 description 1
- 208000008035 Back Pain Diseases 0.000 description 1
- 241000221751 Claviceps purpurea Species 0.000 description 1
- 206010011224 Cough Diseases 0.000 description 1
- 235000017898 Digitaria ciliaris Nutrition 0.000 description 1
- 208000010228 Erectile Dysfunction Diseases 0.000 description 1
- 241000130660 Hepialidae Species 0.000 description 1
- 206010062717 Increased upper airway secretion Diseases 0.000 description 1
- 230000009102 absorption Effects 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 230000000259 anti-tumor effect Effects 0.000 description 1
- 230000003078 antioxidant effect Effects 0.000 description 1
- 208000006673 asthma Diseases 0.000 description 1
- 208000019804 backache Diseases 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000008280 blood Substances 0.000 description 1
- 210000004369 blood Anatomy 0.000 description 1
- 230000009084 cardiovascular function Effects 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 229940126678 chinese medicines Drugs 0.000 description 1
- 208000013116 chronic cough Diseases 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000004069 differentiation Effects 0.000 description 1
- 239000003172 expectorant agent Substances 0.000 description 1
- 230000003419 expectorant effect Effects 0.000 description 1
- 239000003205 fragrance Substances 0.000 description 1
- 230000023597 hemostasis Effects 0.000 description 1
- 201000001881 impotence Diseases 0.000 description 1
- 210000003734 kidney Anatomy 0.000 description 1
- 230000003907 kidney function Effects 0.000 description 1
- 230000003908 liver function Effects 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 210000004072 lung Anatomy 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 206010029410 night sweats Diseases 0.000 description 1
- 230000036565 night sweats Effects 0.000 description 1
- 235000008935 nutritious Nutrition 0.000 description 1
- 208000026435 phlegm Diseases 0.000 description 1
- 238000004321 preservation Methods 0.000 description 1
- 208000008128 pulmonary tuberculosis Diseases 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 238000004781 supercooling Methods 0.000 description 1
- 230000008542 thermal sensitivity Effects 0.000 description 1
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K36/00—Medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicines
- A61K36/06—Fungi, e.g. yeasts
- A61K36/062—Ascomycota
- A61K36/066—Clavicipitaceae
- A61K36/068—Cordyceps
-
- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F26—DRYING
- F26B—DRYING SOLID MATERIALS OR OBJECTS BY REMOVING LIQUID THEREFROM
- F26B5/00—Drying solid materials or objects by processes not involving the application of heat
- 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
- F26B5/06—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 the process involving freezing
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2236/00—Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
- A61K2236/10—Preparation or pretreatment of starting material
- A61K2236/13—Preparation or pretreatment of starting material involving cleaning, e.g. washing or peeling
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2236/00—Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
- A61K2236/10—Preparation or pretreatment of starting material
- A61K2236/17—Preparation or pretreatment of starting material involving drying, e.g. sun-drying or wilting
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- Natural Medicines & Medicinal Plants (AREA)
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- Animal Behavior & Ethology (AREA)
- Biotechnology (AREA)
- Botany (AREA)
- Medical Informatics (AREA)
- Chemical & Material Sciences (AREA)
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- General Health & Medical Sciences (AREA)
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Abstract
The invention discloses a freeze-drying method for cordyceps sinensis. The method comprises the following steps: (1) collecting fresh cordyceps sinensis; (2) removing mud and cleaning; (3) grading; (4) pre-freezing: reducing the room temperature to -40 DEG C in the manner of segmented cooling; (5) sublimation drying: increasing temperature for 0.5h, increasing the temperature of a shelf to -10 DEG C, then performing sublimation drying on cordyceps sinensis at different levels in the manner of increasing temperature according to different programs, and increasing temperature from -10 DEG C to -6 DEG C; (6) desorbing drying; and (7) softening. According to the disclosed provided by the invention, 10kg of cordyceps sinensis can be freeze-dried once; the effects and nutritional ingredients are kept well; the color is from golden yellow to brownish yellow; the satiation rate is excellent; the drying efficiency is high; the cordyceps sinensis is convenient to transport and carry; and the freeze-drying method can be popularized and applied in a large scale.
Description
Invention field
The present invention relates to the technical field that Cordyceps preserve, the side of especially a kind of extensive lyophilization Cordyceps
Method.
Background technology
Cordyceps colonize in bat for section ergot fungus cordyceps sinensis bacterium cordycepssinensis (berk) sacc.
Stroma on hepialidae insect larvae and larva cadaveric complex.According to written by Qing Dynasty name doctor Wu Yi Lip river in 1757 " Bencao Congxin "
Record, the effect of Cordyceps have " protect lung kidney tonifying, hemostasis and phlegm, chronic cough ".Its main product in China Qinghai, Tibet, Sichuan,
Yunnan etc. saves the highland and severe cold grassy marshland of height above sea level 3500～5000m.Cordyceps are for pulmonary tuberculosis, expectorant blood, asthma, night sweat, the soreness of waist
The diseases such as backache, sexual impotence and seminal emission all have preferable curative effect.Modern pharmacology research also shows, Cordyceps have regulation human body to exempt from
The effects such as epidemic disease system, antitumor and antioxidant activity, regulation renal function, recovery liver function, regulation cardiovascular function.
Cordyceps are rare Chinese medicines, but the long term storage of Cordyceps has some moisture absorptions, goes mouldy or nutrition
The problems such as material scatters and disappears.The technology such as the current dry technology for Cordyceps mainly dries, dries, drying in the shade, lyophilization.
But prior art all has some defects, although dry, dry in the shade and dry to carry out on a large scale, Cordyceps can be made
The heat-sensitive nutrition containing and fragrance scatter and disappear, and profile is shrivelled, and appearance color brown stain is serious.The freezing of existing document report is done
Dry technology all can only the small-scale Cordyceps of lyophilizing, be not suitable for the lyophilizing of feather weight sample, authorize within such as 2012 is special
Sharp " a kind of method of rapid freeze-drying of cordyceps sinensis " (cn102178700b), the Cordyceps of each lyophilizing only 100, about 50g
～100g, scale too little it is difficult to realize industrialized production.The success bred with Cordyceps industrialization, a kind of big rule of exploitation
Mould Cordyceps sample freeze drying technology seems very necessary.
Content of the invention
The present invention is directed to disadvantages mentioned above, invents a kind of method of extensive lyophilization Cordyceps, can be good
Preserve thermal sensitivity nutrition and effect material, the full profile of Cordyceps and golden yellow color and luster can be kept moreover it is possible to be applied to work again
Industryization efficiently produces on a large scale.
On the one hand, the present invention provides a kind of cryodesiccated method of Cordyceps, after harvesting fresh Cordyceps
Stripping mud cleans it is characterised in that also including:
(1) be classified: the Cordyceps after cleaning up are classified according to the thickness of homogenizing and weight, 800 with
Under/feather weight be a level, 800-1500 root/feather weight be b level, more than 1500/feather weight be c level；
(2) prefreezing: make temperature drop to -40 DEG C from room temperature in the form of segmentation cooling；
(3) sublimation drying: make shelf temperature rise to -10 DEG C by -40 DEG C, then adopt different temperature programming methods pair
A level, b level or c level Cordyceps carry out sublimation drying, are warmed up to -6 DEG C from -10 DEG C:
To a level Cordyceps: in -10 DEG C of shelf temperature, carry out the regulation of different pressures twice successively, carry out 2 and follow
Ring；When shelf temperature rises to -8 DEG C, carry out the regulation of different pressures twice successively, carry out 3 circulations；Rise again in shelf temperature
During to -6 DEG C, carry out the regulation of different pressures twice successively, carry out 2 circulations；Described different pressures twice are followed successively by 35～
45pa, 10～15pa；
To b level Cordyceps: it is different from the temperature programming method of a level Cordyceps and is, described difference twice is pressed
Power is followed successively by 30～40pa, 10～15pa；
To c level Cordyceps: it is different from the temperature programming method of a level Cordyceps and is, described difference twice is pressed
Power is followed successively by 25～35pa, 5～10pa；
(4) adsorption stripping and dry: shelf temperature is warmed up to 10 DEG C from -6 DEG C；
(5) ease back: by after adsorption stripping and dry Cordyceps take out after humidity range be 60%～85%, temperature range be
Place in 20 DEG C～35 DEG C of space.
In certain embodiments, Cordyceps freeze-drying method of the present invention, the segmentation fall described in its step (2)
The form of temperature is: 0.5h is cooled to -10 DEG C by room temperature；Then 0.5h is cooled to -25 DEG C by -10 DEG C；Last 0.5h is dropped by -25 DEG C
Temperature, to -40 DEG C, is held time as 6-8h.
In certain embodiments, Cordyceps freeze-drying method of the present invention, makes shelf described in its step (3)
Temperature rises to the time used by -10 DEG C for 0.5h by -40 DEG C.
In certain embodiments, Cordyceps freeze-drying method of the present invention, the different journeys described in its step (3)
In sequence temperature-rising method, to a level Cordyceps, when pressure is adjusted to 35～45pa, hold time as 1～2h；When pressure is adjusted
During for 10～15pa, hold time as 3～4h.
In certain embodiments, Cordyceps freeze-drying method of the present invention, the different journeys described in its step (3)
In sequence temperature-rising method, to b level Cordyceps, when pressure is adjusted to 30～40pa, hold time as 1～1.5h；When pressure is adjusted
When saving as 10～15pa, hold time as 2.5-3.5h.
In certain embodiments, Cordyceps freeze-drying method of the present invention, the different journeys described in its step (3)
In sequence temperature-rising method, to c level Cordyceps, when pressure is adjusted to 25～35pa, hold time as 1～1.5h；When pressure is adjusted
When saving as 5～10pa, hold time as 2-3h.
In certain embodiments, Cordyceps freeze-drying method of the present invention, the different journeys described in its step (3)
Sequence temperature-rising method is:
A, a level Cordyceps of less than 800/kilograms: after shelf temperature rises to -10 DEG C, regulation pressure to 35～
45pa, maintains 1～2h, then pressure regulation power, to 10～15pa, maintains 3～4h, carries out 2 circulations；Shelf temperature rises to -8 DEG C, adjusts
Pressure, to 35～45pa, maintains 1～2h, then is adjusted to 10～15pa, maintains 3～4h, carries out 3 circulations；Shelf temperature rises to again-
6 DEG C, adjust pressure to 35～45pa, maintain 1～2h, then be adjusted to 10～15pa, maintain 3～4h, carry out 2 circulations；
B, 800-1500 root/kilogram b level Cordyceps: after shelf temperature rises to -10 DEG C, adjust pressure to 30～
40pa, maintains 1～1.5h, then is adjusted to 10～15pa, maintains 2.5～3.5h, carries out 2 circulations；Shelf temperature rises to -8 DEG C, adjusts
Section pressure, to 30～40pa, maintains 1～1.5h, then is adjusted to 10～15pa, maintains 2.5～3.5h, carries out 3 circulations；Shelf temperature
Degree rises to -6 DEG C again, adjusts pressure to 30～40pa, maintains 1～1.5h, then be adjusted to 10～15pa, maintains 2.5～3.5h, carry out
2 circulations；
C, the c level Cordyceps of more than 1500/kilograms: after shelf temperature rises to -10 DEG C, regulation pressure to 25～
35pa, maintains 1～1.5h, then is adjusted to 5～10pa, maintains 2～3h, carries out 2 circulations；Shelf temperature rises to -8 DEG C, adjusts pressure
Power, to 25～35pa, maintains 1～1.5h, then is adjusted to 5～10pa, maintains 2～3h, carries out 3 circulations；Shelf temperature rises to -6 again
DEG C, adjust pressure to 25～35pa, maintain 1～1.5h, then be adjusted to 5～10pa, maintain 2～3h, carry out 2 circulations.
In certain embodiments, Cordyceps freeze-drying method of the present invention, the described adsorption stripping and dry of its step (4)
For: in 1h, shelf temperature is warmed up to as 10 DEG C from -6 DEG C, pressure is 10pa, then continues 0.8～1.2h.
In certain embodiments, Cordyceps freeze-drying method of the present invention, ease back described in its step (5) process
Time be 20～40min.
Finally, the index of aridity of its finished product is 96%～100%；Full rate is 96%～99%.
In the present invention, the drying of indication refers to Cordyceps water content within 8%, full refers to Cordyceps bar ridge
Network is clear, and no shrivelled shrinkage phenomenon is substantially unchanged before and after lyophilizing.The index of aridity and full rate refer respectively to reach and are dried and full
The ratio of standard.
Beneficial effects of the present invention are as follows:
1. present invention can apply to the extensive lyophilization of Cordyceps, can lyophilizing 5-10kg fresh worm summer in winter
Grass, is applied to extensive commercial application.
2. the present invention is directed to the freeze drying process using differentiation for the fresh Cordyceps of different stage (a, b, c level), can keep away
Exempt from the defect that method different stage Cordyceps degree of drying of the same race differs, largely improve lyophilizing efficiency, save
The energy.
3. the present invention increased the step easing back after lyophilizing, and the Cordyceps after lyophilization are very dry and frangible,
Increasing the process easing back can increase the toughness of Cordyceps, reduce breakdown rate.
4. the present invention takes the mode prefreezing of segmentation cooling, can overcome the technical disadvantages of current prefreezing: existing skill
In art, prefreezing is typically directly down to a certain temperature household freezer temperature, then the Cordyceps after homogenizing is put into household freezer
Middle pre-freeze is for a period of time.In general, rate of cooling is faster, supercooling temperature is lower, and the nucleus quantity of formation is more, and crystal comes not
And growth is just frozen, the resistance that later stage sublimation drying runs into is bigger, and required time is longer.And the side of the segmentation cooling of the present invention
Formula prefreezing, makes temperature be gradually lowered, and the nucleus of formation is big and quantity is relatively fewer, and the resistance that sublimation drying runs into is less, institute
Take time minimizing.
5. the temperature programming of the sublimation drying that the present invention adopts heats up with respect to disposable, has a process, makes drying
Speed be gradually increased, drying is gradually permeated from outside to inside, makes solid-state water sublimate be that vapor is more thorough.
6. the index of aridity of freeze-drying Cordyceps sinensis finished product of the present invention is high, is 96%～100%；Full rate is good, be 96%～
99%, color and luster is pale brown to golden yellow, nutritious, convenient preservation, is easy to carry.
Specific embodiment
In order that the objects, technical solutions and advantages of the present invention become more apparent, below in conjunction with specific embodiment, to this
Invention is further elaborated.It should be appreciated that specific embodiment described herein is only in order to explain the present invention, not
For limiting the present invention.
The freeze-drying method of Cordyceps of the present invention, the embodiment of following mask body is described in more details.
Cordyceps are originated: Yichang mountain city Shui Dou Cordyceps company limited
Carried out front process as follows before sample lyophilizing:
1. harvest fresh Cordyceps；
2. shell mud, cleaning；
3. be classified: the Cordyceps after cleaning up are classified according to the thickness of homogenizing and weight, 800 with
Under/feather weight be a level, 800-1500 root/feather weight be b level, more than 1500/feather weight be c level；
Embodiment 1
The present embodiment adopts the lyo-2 type freeze dryer of Shanghai Tofflon Science and Technology Co., Ltd., lyophilizing 10kg 800
The fresh Cordyceps of a level of below/feather weight, method is:
(1) prefreezing: the fresh a level Cordyceps after harvesting cleaning are made temperature from room temperature in the form of segmentation cooling
Drop to -40 DEG C, its segmentation cooling process is: in the 0.5h time, be cooled to -10 DEG C by room temperature；Then by -10 DEG C in the 0.5h time
It is cooled to -25 DEG C；It is cooled to -40 DEG C by -25 DEG C, hold time 6h in the last 0.5h time；
(2) sublimation drying: the shelf heating-up time is 0.5h, makes shelf temperature rise to -10 DEG C by -40 DEG C, then adopts
The form of temperature programming carries out sublimation drying, is warmed up to -6 DEG C from -10 DEG C.Its temperature programming form is: -10 DEG C of shelf temperature,
Adjust pressure to 35pa, maintain 1h, then be adjusted to 10pa, maintain 3h, carry out 2 circulations；Shelf temperature rises to -8 DEG C, adjusts pressure
To 35pa, maintain 1h, then be adjusted to 10pa, maintain 3h, carry out 3 circulations；Shelf temperature rises to -6 DEG C again, adjust pressure to
35pa, maintains 1h, then is adjusted to 10pa, maintains 3h, carries out 2 circulations；
(3) in adsorption stripping and dry: 1h, shelf temperature is warmed up to as 10 DEG C from -6 DEG C, pressure is 10pa, then the persistent period
0.8h；
(4) ease back: be 20 DEG C in temperature after the Cordyceps of adsorption stripping and dry are taken out, relative air humidity is 60% condition
Under ease back 20min, moisture Control is within 8%.
Finally, the golden yellow color of finished product, the index of aridity is 98%；Full rate is 97%.
Embodiment 2
The present embodiment adopts the lyo-2 type freeze dryer of Shanghai Tofflon Science and Technology Co., Ltd., lyophilizing 10kg 800
The fresh Cordyceps of a level of below/feather weight.
As different from Example 1:
Step (1) prefreezing: make temperature drop to -40 DEG C from room temperature in the form of segmentation cooling, its segmentation cooling process
For: 0.5h is cooled to -10 DEG C in the time；Then it is cooled to -25 DEG C by -10 DEG C in the 0.5h time；By -25 in the last 0.5h time
DEG C it is cooled to -40 DEG C, hold time 8h；
Step (2) sublimation drying: the heating-up time makes shelf temperature rise to -10 DEG C by -40 DEG C for 0.5h, then adopts journey
The form that sequence heats up carries out sublimation drying, is warmed up to -6 DEG C from -10 DEG C.Its temperature programming form is: -10 DEG C of shelf temperature, adjusts
Section pressure, to 45pa, maintains 2h, then is adjusted to 15pa, maintains 4h, carries out 2 circulations；Shelf temperature rises to -8 DEG C, adjust pressure to
45pa, maintains 2h, then is adjusted to 15pa, maintains 4h, carries out 3 circulations；Shelf temperature rises to -6 DEG C again, adjusts pressure to 45pa,
Maintain 2h, then be adjusted to 15pa, maintain 4h, carry out 2 circulations；
In step (3) adsorption stripping and dry: 1h, shelf temperature is warmed up to as 10 DEG C from -6 DEG C, pressure is 10pa, then continues
1.2h；
Step (4) eases back: is 35 DEG C in temperature after the Cordyceps of adsorption stripping and dry are taken out, relative air humidity is 85%
Under the conditions of ease back 40min, moisture Control is within 8%.
Finally, the color and luster of finished product is yellowish-brown, and the index of aridity is 100%；Full rate is 99%.
Embodiment 3
The present embodiment as different from Example 1 the present embodiment adopt Shanghai Tofflon Science and Technology Co., Ltd. lyo-
2 type freeze dryers, the fresh Cordyceps of lyophilizing 10kg b level.
Temperature programming form described in step (2) is: intensification 0.5h makes shelf temperature rise to -10 DEG C by -40 DEG C, adjusts
Pressure, to 30pa, maintains 1h, then is adjusted to 10pa, maintains 2.5h, carries out 2 circulations；Shelf temperature rises to -8 DEG C, adjust pressure to
30pa, maintains 1h, then is adjusted to 10pa, maintains 2.5h, carries out 3 circulations；Shelf temperature rises to -6 DEG C again, adjust pressure to
30pa, maintains 1h, then is adjusted to 10pa, maintains 2.5h, carries out 2 circulations.
Finally, the color and luster of finished product is yellowish-brown, and the index of aridity is 96%；Full rate is 96%.
Embodiment 4
The present embodiment as different from Example 1 the present embodiment adopt Shanghai Tofflon Science and Technology Co., Ltd. lyo-
2 type freeze dryers, the fresh Cordyceps of lyophilizing 10kg b level.
Step (1) prefreezing: make temperature drop to -40 DEG C from room temperature in the form of segmentation cooling, its segmentation cooling process
For: 0.5h is cooled to -10 DEG C in the time；Then it is cooled to -25 DEG C by -10 DEG C in the 0.5h time；By -25 in the last 0.5h time
DEG C it is cooled to -40 DEG C, hold time 8h.
Temperature programming form described in step (2) is: intensification 0.5h makes shelf temperature rise to -10 DEG C by -40 DEG C, adjusts
Pressure, to 40pa, maintains 1.5h, then is adjusted to 15pa, maintains 3.5h, carries out 2 circulations；Shelf temperature rises to -8 DEG C, adjusts pressure
To 40pa, maintain 1.5h, then be adjusted to 15pa, maintain 3.5h, carry out 3 circulations；Shelf temperature rises to -6 DEG C again, adjust pressure to
40pa, maintains 1.5h, then is adjusted to 15pa, maintains 3.5h, carries out 2 circulations.
In step (3) adsorption stripping and dry: 1h, shelf temperature is warmed up to as 10 DEG C from -6 DEG C, pressure is 10pa, then when persistently
Between 1.2h.
Step (4) eases back: is 35 DEG C in temperature after the Cordyceps of adsorption stripping and dry are taken out, relative air humidity is 85%
Under the conditions of ease back 40min, moisture Control is within 8%.
Finally, the color and luster of finished product is yellowish-brown, and the index of aridity is 100%；Full rate is 98%.
Embodiment 5
The present embodiment as different from Example 1 the present embodiment adopt Shanghai Tofflon Science and Technology Co., Ltd. lyo-
2 type freeze dryers, the fresh Cordyceps of lyophilizing 10kg c level.
Temperature programming form described in step (2) is: intensification 0.5h makes shelf temperature rise to -10 DEG C by -40 DEG C, adjusts
Pressure, to 25pa, maintains 1h, then is adjusted to 5pa, maintains 2h, carries out 2 circulations；Shelf temperature rises to -8 DEG C, adjust pressure to
25pa, maintains 1h, then is adjusted to 5pa, maintains 2h, carries out 3 circulations；Shelf temperature rises to -6 DEG C again, adjusts pressure to 25pa, ties up
Hold 1h, then be adjusted to 5pa, maintain 2h, carry out 2 circulations.
Finally, the golden yellow color of finished product, the index of aridity is 96%；Full rate is 96%.
Embodiment 6
The present embodiment as different from Example 1 the present embodiment adopt Shanghai Tofflon Science and Technology Co., Ltd. lyo-
2 type freeze dryers, the fresh Cordyceps of lyophilizing 10kg c level.
Step (1) prefreezing: make temperature drop to -40 DEG C from room temperature in the form of segmentation cooling, its segmentation cooling process
For: 0.5h is cooled to -10 DEG C in the time；Then it is cooled to -25 DEG C by -10 DEG C in the 0.5h time；By -25 in the last 0.5h time
DEG C it is cooled to -40 DEG C, hold time 8h.
Temperature programming form described in step (2) is: intensification 0.5h makes shelf temperature rise to -10 DEG C by -40 DEG C, adjusts
Pressure, to 35pa, maintains 1.5h, then is adjusted to 10pa, maintains 3h, carries out 2 circulations；Shelf temperature rises to -8 DEG C, adjust pressure to
35pa, maintains 1.5h, then is adjusted to 10pa, maintains 3h, carries out 3 circulations；Shelf temperature rises to -6 DEG C again, adjust pressure to
35pa, maintains 1.5h, then is adjusted to 10pa, maintains 3h, carries out 2 circulations.
In step (3) adsorption stripping and dry: 1h, shelf temperature is warmed up to as 10 DEG C from -6 DEG C, pressure is 10pa, then when persistently
Between 1.2h.
Step (4) eases back: is 35 DEG C in temperature after the Cordyceps of adsorption stripping and dry are taken out, relative air humidity is 85%
Under the conditions of ease back 40min, moisture Control is within 8%.
Finally, the color and luster of finished product is yellowish-brown, and the index of aridity is 99%；Full rate is 98%.
Embodiment 7
The present embodiment adopts the lyo-2 type freeze dryer of Shanghai Tofflon Science and Technology Co., Ltd., and lyophilizing 10kg is not carried out
The fresh Cordyceps (comprising a, b and c Three Estate) of staged care, method is:
(1) prefreezing: the fresh unassorted fresh Cordyceps after harvesting cleaning are dropped to -40 DEG C from room temperature, maintains
Time 8h；
(2) sublimation drying: the shelf heating-up time is 0.5h, makes shelf temperature rise to -10 DEG C by -40 DEG C, adjusts pressure
To 10pa, then it is vacuum dried 80h at -10 DEG C；
(3) in adsorption stripping and dry: 1h, shelf temperature is warmed up to 10 DEG C from -6 DEG C, pressure is 10pa, then persistent period 0.8h；
(4) ease back: be 20 DEG C in temperature after the Cordyceps of adsorption stripping and dry are taken out, relative air humidity is 65% condition
Under ease back 20min, moisture Control is within 8%.
Finally, the golden yellow color of finished product, the index of aridity is 97%；Full rate is 98%.
Embodiment discussion of results:
By embodiment 1-7 contrast display (being shown in Table 1), embodiment 7 adopts conventional prefreezing, sublimation drying, and not to the winter
Worm summer grass carry out staged care so that the 10kg Cordyceps index of aridity reach more than 98% need time-consuming be up to 90 hours, and this
Invention is on the basis of be classified to Cordyceps size, then the prefreezing in the form of being lowered the temperature using segmentation, temperature programming
The method of sublimation drying, greatly improves lyophilizing efficiency, time-consuming 31.1-54.8 hour can 10 kilograms of lyophilizing the fresh worm summer in winter
Grass.
The contrast of table 1 embodiment 1-7
Certainly, the present invention also can have other various embodiments, in the case of without departing substantially from present invention spirit and its essence, ripe
Know those skilled in the art and work as and various corresponding changes and deformation can be made according to the present invention, but these corresponding changes and change
Shape all should belong to the protection domain of appended claims of the invention.
Claims (9)
1. a kind of Cordyceps freeze-drying method, including stripping mud cleaning after harvesting fresh Cordyceps it is characterised in that going back
Including:
(1) it is classified: the Cordyceps after cleaning up are classified according to the thickness of homogenizing and weight, less than 800/public
Jin level is a level, 800-1500 root/feather weight is b level, more than 1500/feather weight is c level；
(2) prefreezing: make temperature drop to -40 DEG C from room temperature in the form of segmentation cooling；
(3) sublimation drying: make shelf temperature rise to -10 DEG C by -40 DEG C；
Then sublimation drying is carried out to a level, b level or c level Cordyceps using different temperature programming methods, heat up from -10 DEG C
Arrive -6 DEG C:
To a level Cordyceps: in -10 DEG C of shelf temperature, carry out the regulation of different pressures twice successively, carry out 2 circulations；?
When shelf temperature rises to -8 DEG C, carry out the regulation of different pressures twice successively, carry out 3 circulations；Rise to -6 in shelf temperature again
DEG C when, carry out the regulation of different pressures twice successively, carry out 2 circulation；Described different pressures twice be followed successively by 35～45pa,
10～15pa；
To b level Cordyceps: it is different from the temperature programming method of a level Cordyceps and is, described different pressures twice according to
Secondary is 30～40pa, 10～15pa；
To c level Cordyceps: it is different from the temperature programming method of a level Cordyceps and is, described different pressures twice according to
Secondary is 25～35pa, 5～10pa；
(4) adsorption stripping and dry: shelf temperature is warmed up to 10 DEG C from -6 DEG C；
(5) ease back: by after adsorption stripping and dry Cordyceps take out after humidity range be 60%～85%, temperature range be 20 DEG C
Place in～35 DEG C of space.
2. Cordyceps freeze-drying method according to claim 1 is it is characterised in that the segmentation described in step (2) is dropped
The form of temperature is: is cooled to -10 DEG C by room temperature in 0.5h；Then it is cooled to -25 DEG C by -10 DEG C in 0.5h；In last 0.5h by-
25 DEG C are cooled to -40 DEG C, and hold time 6-8h.
3. Cordyceps freeze-drying method according to claim 1 is it is characterised in that make shelf described in step (3)
Temperature rises to the time used by -10 DEG C for 0.5h by -40 DEG C.
4. Cordyceps freeze-drying method according to claim 1 is it is characterised in that different described in step (3)
In temperature programming method, to a level Cordyceps, when pressure is adjusted to 35～45pa, hold time as 1～2h；When pressure is adjusted
When saving as 10～15pa, hold time as 3～4h.
5. Cordyceps freeze-drying method according to claim 1 is it is characterised in that different described in step (3)
In temperature programming method, to b level Cordyceps, when pressure is adjusted to 30～40pa, hold time as 1～1.5h；Work as pressure
When being adjusted to 10～15pa, hold time as 2.5-3.5h.
6. Cordyceps freeze-drying method according to claim 1 is it is characterised in that different described in step (3)
In temperature programming method, to c level Cordyceps, when pressure is adjusted to 25～35pa, hold time as 1～1.5h；Work as pressure
When being adjusted to 5～10pa, hold time as 2-3h.
7. Cordyceps freeze-drying method according to claim 1 is it is characterised in that different described in step (3)
Temperature programming method is:
A, a level Cordyceps of less than 800/kilograms: after shelf temperature rises to -10 DEG C, adjust pressure to 35～45pa, tie up
Hold 1～2h, then pressure regulation power, to 10～15pa, maintains 3～4h, carries out 2 circulations；Shelf temperature rises to -8 DEG C, adjust pressure to
35～45pa, maintains 1～2h, then is adjusted to 10～15pa, maintains 3～4h, carries out 3 circulations；Shelf temperature rises to -6 DEG C again, adjusts
Section pressure, to 35～45pa, maintains 1～2h, then is adjusted to 10～15pa, maintains 3～4h, carries out 2 circulations；
B, 800-1500 root/kilogram b level Cordyceps: after shelf temperature rises to -10 DEG C, adjust pressure to 30～40pa,
Maintain 1～1.5h, then be adjusted to 10～15pa, maintain 2.5～3.5h, carry out 2 circulations；Shelf temperature rises to -8 DEG C, adjusts pressure
Power, to 30～40pa, maintains 1～1.5h, then is adjusted to 10～15pa, maintains 2.5～3.5h, carries out 3 circulations；Shelf temperature is again
Rise to -6 DEG C, adjust pressure to 30～40pa, maintain 1～1.5h, then be adjusted to 10～15pa, maintain 2.5～3.5h, carry out 2
Circulation；
C, the c level Cordyceps of more than 1500/kilograms: after shelf temperature rises to -10 DEG C, adjust pressure to 25～35pa,
Maintain 1～1.5h, then be adjusted to 5～10pa, maintain 2～3h, carry out 2 circulations；Shelf temperature rises to -8 DEG C, regulation pressure to 25
～35pa, maintains 1～1.5h, then is adjusted to 5～10pa, maintains 2～3h, carries out 3 circulations；Shelf temperature rises to -6 DEG C again, adjusts
Section pressure, to 25～35pa, maintains 1～1.5h, then is adjusted to 5～10pa, maintains 2～3h, carries out 2 circulations.
8. Cordyceps freeze-drying method according to claim 1 is it is characterised in that the described adsorption stripping and dry of step (4)
For: in 1h, shelf temperature is warmed up to 10 DEG C from -6 DEG C, pressure is 10pa, then continues 0.8～1.2h.
9. Cordyceps freeze-drying method according to claim 1 is it is characterised in that the process that eases back described in step (5)
Time be 20～40min.
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| CN109916141A (en) * | 2019-01-31 | 2019-06-21 | 武汉科技大学 | A kind of low temperature dewatering processing method for metallurgical alloy powder |
| CN109984184A (en) * | 2019-05-21 | 2019-07-09 | 新疆黑果枸杞生物科技有限公司 | A kind of freeze-drying method of small white almond |
| CN112089746A (en) * | 2019-06-18 | 2020-12-18 | 贵州广济堂药业有限公司 | Traditional Chinese medicine wall-broken decoction pieces and raw material processing method and preparation method thereof |
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| CN112090557A (en) * | 2019-06-18 | 2020-12-18 | 贵州广济堂药业有限公司 | Traditional Chinese medicine wall-broken decoction pieces and raw material crushing method and preparation method thereof |
| CN112213431A (en) * | 2019-07-10 | 2021-01-12 | 贵州广济堂药业有限公司 | Detection method and quality control method of rhodiola rosea wall-broken decoction pieces |
| CN112206248A (en) * | 2019-07-10 | 2021-01-12 | 贵州广济堂药业有限公司 | Rhodiola wall-breaking decoction piece and preparation method and application thereof |
| CN113521116A (en) * | 2021-08-18 | 2021-10-22 | 东莞市东阳光冬虫夏草研发有限公司 | Cordyceps sinensis composition and preparation method thereof |
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Denomination of invention: Freeze-drying method for cordyceps sinensis Effective date of registration: 20190903 Granted publication date: 20190524 Pledgee: Yichang Branch of Bohai Bank Co., Ltd.|Three Gorges Branch of Bank of China Co., Ltd.|Nanhu Branch of Hubei Bank Co., Ltd.|Yichang Branch of Hankou Bank Co., Ltd. Pledgor: Guangdong Dongguang Sunshine Pharmaceutical Co., Ltd.|Yichang Shancheng Shuidu Cordyceps sinensis Co., Ltd. Registration number: Y2019420000010 |
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Denomination of invention: Freeze drying method of Cordyceps sinensis Effective date of registration: 20200902 Granted publication date: 20190524 Pledgee: Bank of Bohai Limited by Share Ltd. Yichang branch|Bank of China Limited by Share Ltd. Three Gorges Branch|Bank of Hubei Limited by Share Ltd. Yichang Nanhu sub branch|Bank of Hankou Limited by Share Ltd. Yichang branch Pledgor: YICHANG SHANCHENGSHUIDU CORDYCEPS Co.,Ltd. Registration number: Y2020420000061 |
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