CN106692703A - Preparation method of dendrobium freeze-dried powder - Google Patents
Preparation method of dendrobium freeze-dried powder Download PDFInfo
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- CN106692703A CN106692703A CN201710159994.5A CN201710159994A CN106692703A CN 106692703 A CN106692703 A CN 106692703A CN 201710159994 A CN201710159994 A CN 201710159994A CN 106692703 A CN106692703 A CN 106692703A
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- 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
- A61K36/18—Magnoliophyta (angiosperms)
- A61K36/88—Liliopsida (monocotyledons)
- A61K36/898—Orchidaceae (Orchid family)
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- A61K9/14—Particulate form, e.g. powders, Processes for size reducing of pure drugs or the resulting products, Pure drug nanoparticles
- A61K9/19—Particulate form, e.g. powders, Processes for size reducing of pure drugs or the resulting products, Pure drug nanoparticles lyophilised, i.e. freeze-dried, solutions or dispersions
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- 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
- A61K2236/15—Preparation or pretreatment of starting material involving mechanical treatment, e.g. chopping up, cutting or grinding
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- 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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Abstract
The invention provides a preparation method of dendrobium freeze-dried powder. The preparation method comprises the following steps: firstly, breaking walls of a dendrobium raw material by adopting an ultrahigh pressure low temperature technique; secondly, grinding the dendrobium raw material after the walls are broken into thick liquid and uniformly mixing, and carrying out vacuum freeze-drying, so that dendrobium powder is obtained, wherein the vacuum freeze-drying process concretely comprises that pre-freezing, primary sublimation and secondary sublimation are sequentially carried out on the dendrobium raw material after being ground into the thick liquid and uniformly mixed; and thirdly, carrying out superfine grinding on dendrobium powder. In the preparation method of the dendrobium freeze-dried powder, the ultrahigh pressure low temperature technique is adopted for breaking the walls, and the vacuum freeze-drying and the superfine grinding are combined, so that raw material utilization ratio is improved, the biological activity of functional substances in fresh dendrobium raw materials is hardly lost, and pharmaceutical values and health effects of the dendrobium raw materials are enhanced.
Description
Technical field
The present invention relates to processing technique of Chinese herbs field, a kind of preparation method of stem of noble dendrobium freeze-dried powder is specifically related to.
Background technology
Fresh medicine refers to the tissue in whole or in part with fresh plant or animal, or takes the medicine that its juice working process is made
Thing, using the method for fresh medicine in addition to entering decoction, often takes from right juice and takes.The Ming Dynasty《Compendium of Materia Medica》In just have 1100 a plurality of
Using the subsidiary formula of fresh medicine, the application of ancient times fresh medicine reaches a summit.To the modern times, due to the culture of fresh medicine, storage and transport
It is defeated relatively costly, the limitation of process technology is added, the fresh-keeping difficulty of fresh medicine limits its application clinically, the application of fresh medicine
The trend of gradually atrophy is presented, fails to be developed.Fresh medicine is mainly clinically replaced with dry product at present, and traditional process technology
The loss of fresh medicine active component can be caused so that the pharmacological action reduction of fresh medicine material, it is impossible to adapt to clinical demand.Wherein key is asked
Topic is fresh medicine in storage, processing, transport and using upper extremely inconvenient, and perishable failure, also can using conventional machining techniques
Its nutritional ingredient is reduced, using new processing method, to solve its transport, very necessary using upper inconvenience.
The stem of noble dendrobium is orchid family herbaceous plant, principle active component be water-soluble polysaccharide, interior lipo-alkaloids, free amino acid with
And various trace elements etc., immune function of human body can be improved, with enriching yin, removing toxic substances, anticancer, antifatigue, radioresistance, resist oxygen lack,
Anti-aging etc. is acted on.When the medical stem of noble dendrobium " in, be particular about fresh goods for upper ", often takes from right juice and takes, and natural juice maintains crude drug
Original nature and flavor of thing, smell is all deposited, the characteristics of the property moisturized of tool is stronger.2010 editions《Chinese Pharmacopoeia》Also by air-dried Dendrobium and fresh goods
Separate introduction.Chinese department of traditional Chinese medicine institute professor Hao Jin great research finds, fresh dendrobium total alkaloids, many compared with air-dried Dendrobium
Sugared content is above dry product, and it improves immunologic function also superior to dry medicine, the characteristics of also demonstrate the stem of noble dendrobium " survivor is excellent ".And it is current
The process of the in the market stem of noble dendrobium is substantially needed by arranging, bakeing, curling adds hoop, dry 4 processing steps, is entirely being processed
Link, the nutriment for being related to bake and bank up with earth and dry inherently to some thermal sensitivity produces destruction, or reduces its content.
The content of the invention
In view of this, a kind of preparation method of stem of noble dendrobium freeze-dried powder that the present invention is provided, preferably overcomes above-mentioned existing skill
Problem and defect that art is present, are combined, no by using super-pressure cryogenic technique broken wall, vacuum freeze drying and ultramicro grinding
Improve only raw material availability, and the bioactivity for possessing functional materials in fresh stem of noble dendrobium raw material is hardly damaged
Lose, strengthen its medical value and health-care efficacy.
A kind of preparation method of stem of noble dendrobium freeze-dried powder, comprises the following steps：
Step one, broken wall is carried out to fresh stem of noble dendrobium raw material using super-pressure cryogenic technique；
Step 2, by the stem of noble dendrobium raw material after broken wall by defibrination mixing after, dendrobe powder is obtained using vacuum freeze drying；Institute
Vacuum freeze drying process is stated to specifically include：Stem of noble dendrobium raw material after defibrination is mixed carry out successively precooling, for the first time distillation and
Distil for second；
Step 3, dendrobe powder is carried out into ultramicro grinding treatment.
Further, the stem of noble dendrobium raw material is selected from Dendrobium Moniliforme, Herba Dendrobii, HERBA DENDROBII, stem of Eyeshaped Dendrobium, globe daisy stone
One kind in dry measure used in former times, dendrobium, dendrobium loddigesii Rolfe and purple dendrobium；The stem of noble dendrobium raw material is the biennial fresh stem of noble dendrobium.
Further, also include selecting without damaged without the stem of noble dendrobium for going mouldy before the step one, and remove blade and cleaning.
Further, in the step one, the super-pressure cryogenic technique condition is specifically included：Pressure be 450~
550MPa, 1~3min of pressurize；Temperature is 40~60 DEG C.
Further, in the step 2, stem of noble dendrobium granularity is made to be less than 10 μm after the defibrination.
Further, in the step 2, the condition of the precooling includes：By the outlet of the pump of vacuum freeze drier
Pressure is set to 0.05~0.1Mpa；Control material thickness is 10~20mm, and precooling temperature is -35 DEG C~-40 DEG C, precooling
Time is 2~2.5h.
Further, in the step 2, the condition of the first time distillation includes：Control material thickness be 10~
20mm, pressure is 55~65Pa, and when drying temperature is 40~50 DEG C, drying time is 10~12h.
Further, in the step 2, the condition of second distillation includes：Control material thickness be 10~
20mm, 55~65Pa of pressure, drying temperature are 50~60 DEG C, and drying time is 1.5~2h.
Further, in the step 2, also include that it is 10~15Pa/ to set leakage pressure after second distillation
Min is lost heart, and then proceedes to dry 2~3h at 50~60 DEG C.
Further, in the step 3,60 mesh sieves were also included after dendrobe powder is carried out into ultramicro grinding.
Compared with prior art, a kind of beneficial effect of the preparation method of stem of noble dendrobium freeze-dried powder that the present invention is provided is：
(1) preparation method of stem of noble dendrobium freeze-dried powder of the invention uses super-pressure cryogenic technique broken wall, makes fresh stem of noble dendrobium cell
Wall, cell membrane lysis, abundant release medicinal composition simultaneously keep the activity of medicinal ingredient, while also can well protect the stem of noble dendrobium vivid
Color and luster；Using Vacuum Freezing ＆ Drying Technology combination superfine communication technique, the full effect for realizing the stem of noble dendrobium is utilized.Simultaneously as product
It is ultra-micro powder, powder particle is small, surface area is big, absorbs faster, purposes is more extensive, can be used as medicine directly as the prepared slices of Chinese crude drugs,
Can expect as the first wife of other food, health products, medicine.
(2) stem of noble dendrobium method for preparing freeze-dried powder of the invention is simple, and the life of functional materials is possessed in fresh stem of noble dendrobium raw material
Thing activity is hardly suffered a loss, and without any chemical reagent in preparation process, does not have solvent contamination or residual, more day
So, the health theory of modern people is more met.
Specific embodiment
For the ease of understanding the present invention, technical scheme is elaborated with reference to the mode of embodiment,
Elaborate many details in order to fully understand the present invention in the following description.
But the present invention can be implemented with being much different from other manner described here, those skilled in the art can be with
Similar improvement is done in the case of without prejudice to intension of the present invention, therefore the present invention is not limited by following public specific implementation.
Unless otherwise defined, all technologies used herein and scientific terminology have and the common skill of art of the present invention
The identical implication that art personnel are generally understood that.When there is contradiction, the definition in this specification is defined.
Term as used herein：
" by ... prepare " it is synonymous with "comprising".Term "comprising" used herein, " including ", " having ", " containing "
Or its any other deformation, it is intended that cover including for non-exclusionism.For example, composition, step, method comprising listed elements,
Product or device are not necessarily limited to those key elements, and can be including not expressly listed other key elements or this kind of composition, step
Suddenly, method, product or the intrinsic key element of device.
Conjunction " by ... constitute " exclude any key element do not pointed out, step or component.If be used in claim,
This phrase will make claim be closed, it is not included the material in addition to the material that those are described, but relative
Except customary impurities.When phrase " by ... constitute " be rather than immediately following after theme in the clause that appears in claim main body
When, it is only limited to the key element described in the clause；Other key elements be not excluded as the overall claim it
Outward.
Equivalent, concentration or other values or parameter are excellent with scope, preferred scope or a series of upper limit preferred values and lower limit
During the Range Representation that choosing value is limited, this is appreciated that and specifically discloses by any range limit or preferred value and any scope
All scopes that any pairing of lower limit or preferred value is formed, regardless of whether whether the scope separately discloses.For example, when open
During scope " 1~5 ", described scope should be interpreted as including scope " 1~4 ", " 1~3 ", " 1~2 ", " 1~2 and 4~
5 ", " 1~3 and 5 " etc..When number range is described herein, unless otherwise indicated, otherwise the scope is intended to include its end
Value and all integers and fraction within the range.
"and/or" is used to represent that one of illustrated situation or both may to occur, for example, A and/or B includes (A
And B) and (A or B)；
Additionally, the indefinite article " one kind " and " one " before key element of the present invention or component are to key element or the quantitative requirement of component
(i.e. occurrence number) unrestriction.Therefore " one " or " one kind " should be read as including one or at least one, and odd number
The key element or component of form also include plural form, unless the quantity refers to substantially singulative.
In addition, the statement of " at least one " herein include one and the above all numbers (for example, at least 2, at least
4, at least 6, at least 8, at least 10, at least 25, at least 50, at least 100 etc.).
The invention provides a kind of preparation method of stem of noble dendrobium freeze-dried powder, comprise the following steps：
Step one, broken wall is carried out to fresh stem of noble dendrobium raw material using super-pressure cryogenic technique；
Step 2, by the broken wall after fresh stem of noble dendrobium raw material by defibrination mixing after, obtained using vacuum freeze drying
Dendrobe powder；The vacuum freeze drying process is specifically included：Stem of noble dendrobium raw material after defibrination is mixed carries out precooling, first successively
Secondary distillation and second distillation；
Step 3, dendrobe powder is carried out into ultramicro grinding treatment.
The preparation method of stem of noble dendrobium freeze-dried powder of the invention use super-pressure cryogenic technique broken wall, make fresh stem of noble dendrobium cell membrane,
Cell membrane lysis, abundant release medicinal composition simultaneously keeps the activity of medicinal ingredient, while also can well protect the vivid color of the stem of noble dendrobium
Pool；Using Vacuum Freezing ＆ Drying Technology combination superfine communication technique, the full effect for realizing the stem of noble dendrobium is utilized.Simultaneously as product is
Ultra-micro powder, powder particle is small, and surface area is big, absorbs faster, and purposes is more extensive, can be used as medicine directly as the prepared slices of Chinese crude drugs, also may be used
First wife as other food, health products, medicine expects.
Preferably, the stem of noble dendrobium raw material be selected from Dendrobium Moniliforme, Herba Dendrobii, HERBA DENDROBII, stem of Eyeshaped Dendrobium, Dendrobium thyrsiflorum,
One kind in dendrobium, dendrobium loddigesii Rolfe and purple dendrobium；The stem of noble dendrobium raw material is the biennial fresh stem of noble dendrobium.
Above-mentioned, Dendrobium Moniliforme originates from Lijiang, yunnan city Huaping County, the fresh stem of noble dendrobium；Herba Dendrobii originates from Ziyun County, Guizhou Province,
The fresh stem of noble dendrobium；HERBA DENDROBII originates from Xingyi City, Guizhou Province, the fresh stem of noble dendrobium；Stem of Eyeshaped Dendrobium is called Dendrobium fimbriatum Hook, originates from Baise of Guangxi
City, the fresh stem of noble dendrobium；Dendrobium thyrsiflorum originates from Yunnan Puer City, the fresh stem of noble dendrobium；Dendrobium originates from Guangxi region, the fresh stem of noble dendrobium；Ring
The careless stem of noble dendrobium originates from Xingyi City, Guizhou Province, the fresh stem of noble dendrobium；Purple dendrobium originates from Lijiang, yunnan city Huaping County, the fresh stem of noble dendrobium.
Dendrobium Moniliforme, also known as：Dendrobium moniliformeSweet, thin yellow grass belongs to orchid family Dendrobium, and perennial draft of growing nonparasitically upon another plant is a kind of rare
Chinese herbal medicine, with high medicinal health value.In Dendrobium Moniliforme containing various chemistry such as polysaccharide higher, TA into
Part, modern pharmacological research more prove Dendrobium Moniliforme have reinforcing stomach reg fluid, nourishing Yin and clearing heat, support voiceless sound improving eyesight, antitumor, anti-aging,
The effects such as radioresistance, enhancing body immunity.
HERBA DENDROBII is the stem of orchid, and cold nature is sweet, with reinforcing stomach reg fluid, nourishing Yin and clearing heat.For impairment of yin Tianjin
Thanks to, dry polydipsia, deficiency of food is retched, after being ill abnormal heat, and mesh is secretly failed to understand.HERBA DENDROBII chemical composition is mainly containing stem of noble dendrobium Huang alkali, modern medicine
Reason research shows：Dendrobine is that pancreas islet supplements enough nutrition, and acute activation insulin β cells secrete substantial amounts of insulin, drop
Hypoglycemia, while the acceptor on active cell surface again, makes the sugar in blood smoothly into cell and be used, solves pancreas islet
Plain resistance problem.
Herba Dendrobii is a mutation of the orchid family Dendrobium Sw line leaf stem of noble dendrobium, sweet, is slightly cold, and returns stomach, kidney channel, with benefit
Stomach promotes the production of body fluid, effect of nourishing Yin and clearing heat.For impairment of yin body fluid deficiency, dry polydipsia, the after being ill card such as abnormal heat.Herba Dendrobii chemical composition is main
There are polysaccharide, bibenzyl, sequiterpene, cumarin, steroidal etc., wherein polysaccharide is main component.Polysaccharide have enhancing immunity of organisms,
Hypoglycemic, antitumor, anti-aging, anti-oxidant etc. act on.
Stem of Eyeshaped Dendrobium is traditional rare traditional Chinese medicine.《Sheng Nong's herbal classic》In it is on the books, its have reinforcing stomach reg fluid, enriching yin give birth to
The effects such as Tianjin, clearing and antitussive moistening lung.Modern pharmacological research shows, the stem of noble dendrobium is also antitumor, anti-aging, enhancing body immunity and
The effect of expansion of blood vessels.
The effects such as Dendrobium thyrsiflorum has nourishing Yin and clearing heat, the beneficial stomach that promotes the production of body fluid, moistens the lung and relieve the cough, is tired of for treating consumption of body fluid caused by febrile disease, dry
Yearningly, various disease conditions such as abnormal heat after being ill.Isolated Fluorenone class, bibenzyl, luxuriant and rich with fragrance class and flavonoids 13 are extracted from Dendrobium thyrsiflorum
Compound, rich in cumarin.Experimental studies have found that there are cumarin various pharmacology such as AntiHIV1 RT activity, antitumor, anti-oxidant, anti-inflammatory to live
Property, clinically it is widely used in the treatment of anticoagulation and lymphatic edema.
Dendrobium is orchid family Dendrobium Sw, alias HERBA DENDROBII, yellow grass.Modern study shows that its acidic polysaccharose has
There is certain Immune enhancement and antitumor action, it has also become one of main substitute of the stem of noble dendrobium, quilt《Guizhou Province's Chinese medicine standard》
(1988 editions) and《Jiangsu Province's Chinese medicine standard》(1988 editions) are recorded.Dendrobium chrysanthemum triphenol is natural products, bioavilability
High, Nature comparison stabilization, with Clinical practice value.
Dendrobium loddigesii Rolfe is also named that Dendrobium loddigesii, lofty or bottomless palpus, small ring be careless, small yellow grass, is the stem of orchid dendrobium loddigesii Rolfe.Nature and flavor
It is sweet, be slightly cold, return stomach, lung channel, kidney channel, can promote the production of body fluid beneficial stomach；Nourishing Yin and clearing heat；Moistening lung kidney-nourishing；The strong waist of improving eyesight.Stem contains shihunine,
The alkaloids such as shihunidine alkali, dendrophnol.Dendrobine has a liter hyperglycaemia, reduces blood pressure, weakens cardiac contractile force, and dendrobine has one
Fixed analgesic antipyretic effect, it is similar to phenaetin and weaker.
Purple dendrobium is orchid dendrobium devonianum, is slightly cold, sweet, returns stomach, kidney channel.Traumatic injury is controlled in external application, the injury of the tissues of fracturing；
It is for oral administration to control throat and itch, cough.With reinforcing stomach reg fluid, effect of nourishing Yin and clearing heat, for impairment of yin body fluid deficiency, the tired purple dendrobium of dry is thirsty,
Deficiency of food is retched, after being ill abnormal heat, and mesh is secretly failed to understand.It also has certain antipyretic effect, can promote gastric secretion, aid digestion, there is increasing
Excitometabolic, the anti-ageing effect of waiting for a long time.At 2005 editions《Chinese Pharmacopoeia》In, only dendrobium candidum, the purple dendrobium mainly included
With three kinds of stem of noble dendrobium class plants of firm arthrolith dry measure used in former times, wherein clinical best with the medical value of dendrobium candidum and purple dendrobium.
Preferably, also include selecting without damaged without the stem of noble dendrobium for going mouldy before the step one, and remove blade and cleaning.
Preferably, in the step one, the super-pressure cryogenic technique condition is specifically included：Pressure is 450~550MPa
Such as 450MPa, 480MPa, 500MPa, 520MPa or 550MPa, 1~3min of pressurize such as 1min, 2min or 3min etc.；Temperature is
40~60 DEG C such as 40 DEG C, 45 DEG C, 50 DEG C, 55 DEG C or 60 DEG C.
Preferably, in the step 2, stem of noble dendrobium granularity is made to be less than 10 μm after the defibrination.
Preferably, in the step 2, the condition of the precooling includes：By the outlet pressure of the pump of vacuum freeze drier
Power is set to 0.05~0.1Mpa such as 0.05Mpa, 0.06Mpa, 0.07Mpa, 0.08Mpa, 0.09Mpa or 0.1Mpa etc.；Control
Material thickness is 10~20mm such as 10mm, 12mm, 15mm, 18mm or 20mm etc., and precooling temperature is -35 DEG C~-40 DEG C such as -35
DEG C, -36 DEG C, -37 DEG C, -38 DEG C, -39 DEG C or -40 DEG C, the precooling time be 2~2.5h such as 2h, 2.1h, 2.2h, 2.3h, 2.4h
Or 2.5h.
Preferably, in the step 2, the condition of the first time distillation includes：Control material thickness is 10~20mm,
Pressure is 55~65Pa, and drying temperature is 40~50 DEG C such as 40 DEG C, 42 DEG C, 45 DEG C, -48 DEG C or 50 DEG C, and drying time is 10
~12h such as 10h, 10.5h, 11h, 11.5h or 12h.
Preferably, in the step 2, the condition of second distillation includes：Control material thickness be 10~20mm such as
10mm, 12mm, 15mm, 18mm or 20mm etc., 55~65Pa of pressure such as 55Pa, 56Pa, 57Pa, 58Pa, 59Pa or 60Pa etc., do
Dry temperature be 50~60 DEG C such as 50 DEG C, 52 DEG C, 55 DEG C, 58 DEG C or 60 DEG C, drying time be 1.5~2h such as 1.5h, 1.6h,
1.7h, 1.8h, 1.9h or 2h.
Preferably, in the step 2, also include that it is 10~15Pa/min to set leakage pressure after second distillation
Lost heart during such as 10Pa/min, 11Pa/min, 12Pa/min, 13Pa/min, 14Pa/min or 15Pa/min, then proceeded to
2~3h such as 2h, 2.2h, 2.5h, 2.8h or 3h are dried at 50~60 DEG C such as 50 DEG C, 52 DEG C, 55 DEG C, 58 DEG C or 60 DEG C.
Preferably, in the step 3,60 mesh sieves were also included after dendrobe powder is carried out into ultramicro grinding.
For the ease of understanding the present invention, technical scheme is further illustrated with reference to embodiment.Applicant
Statement, the present invention illustrates detailed process equipment of the invention and technological process by above-described embodiment, but the present invention not office
It is limited to above-mentioned detailed process equipment and technological process, that is, does not mean that the present invention should rely on above-mentioned detailed process equipment and technique stream
Cheng Caineng is implemented.Person of ordinary skill in the field it will be clearly understood that any improvement in the present invention, to each original of product of the present invention
Addition, selection of concrete mode of the equivalence replacement and auxiliary element of material etc., all fall within protection scope of the present invention and open model
Within enclosing.
Embodiment 1
A kind of preparation method of stem of noble dendrobium freeze-dried powder, comprises the following steps：
Step one, stem of noble dendrobium raw material are checked and accepted：Dendrobium Moniliforme originates from Lijiang, yunnan city Huaping County, the fresh stem of noble dendrobium.
Step 2, select and clean：Select without damaged without the stem of noble dendrobium for going mouldy, and remove blade；Then pure water rinsing stone is used
Dry measure used in former times.
Step 3, broken wall：Using super-pressure cryogenic technique, make stem of noble dendrobium cell membrane, cell membrane lysis, abundant release medicinal into
Divide and keep the activity of medicinal ingredient, can well protect the vivid color and luster of the stem of noble dendrobium.Super-pressure cryogenic technique treatment conditions are：Super
The cold water of the built-in certain volume of high-pressure bottle, container pressure is 450MPa, and pressurize 1min, temperature is 60 DEG C.
Step 4, defibrination are mixed：It is using fiberizer that the stem of noble dendrobium raw material after step 3 broken wall is levigate, it is less than stem of noble dendrobium granularity
10 μm, then mix.
Step 5, vacuum freeze drying：
(1) precooling：The outlet pressure of controlling pump is 0.05Mpa, opens compressor and plate low temperature valve, and control material thickness is
10mm；It is -35 DEG C to set precooling temperature, and the precooling time is 2.5h.
(2) distil for the first time：Plate low temperature valve is closed, vavuum pump is opened, control material thickness is 10mm；Setting pressure is
55Pa, temperature of heating plate is 50 DEG C, and drying time is 10h.
(3) distil for second：Control material thickness is 10mm；Setting pressure is 55Pa, and temperature of heating plate is 60 DEG C, constant temperature
1.5h is dried, material moisture is controlled within 5%.
(4) lose heart：Leakage pressure is set for 10Pa/min is lost heart.
(5) lose heart after terminating, continue the freeze-day with constant temperature 3h at 50 DEG C, freeze-drying process terminates.
Step 6, crushing：Crushed using micronizer, crossed 60 mesh sieves, obtained the homogeneous powdered stem of noble dendrobium of quality thin
Powder finished product.
Step 7, packaging：Nitrogen-filled packaging sealing is carried out in time to the stem of noble dendrobium freeze-dried powder after above-mentioned crushing, and is put in storage preservation.
Embodiment 2
A kind of preparation method of stem of noble dendrobium freeze-dried powder, comprises the following steps：
Step one, stem of noble dendrobium raw material are checked and accepted：Herba Dendrobii originates from Ziyun County, Guizhou Province, the fresh stem of noble dendrobium.
Step 2, select and clean：Select without damaged without the stem of noble dendrobium for going mouldy, and remove blade；Then pure water rinsing stone is used
Dry measure used in former times.
Step 3, broken wall：Using super-pressure cryogenic technique, make stem of noble dendrobium cell membrane, cell membrane lysis, abundant release medicinal into
Divide and keep the activity of medicinal ingredient, can well protect the vivid color and luster of the stem of noble dendrobium.Super-pressure cryogenic technique treatment conditions are：Super
The cold water of the built-in certain volume of high-pressure bottle, container pressure is 480MPa, and pressurize 2min, temperature is 55 DEG C.
Step 4, defibrination are mixed：It is using fiberizer that the stem of noble dendrobium raw material after step 3 broken wall is levigate, it is less than stem of noble dendrobium granularity
10 μm, then mix.
Step 5, vacuum freeze drying：
(1) precooling：The outlet pressure of controlling pump is 0.06Mpa, opens compressor and plate low temperature valve, and control material thickness is
10mm；It is -36 DEG C to set precooling temperature, and the precooling time is 2.4h.
(2) distil for the first time：Plate low temperature valve is closed, vavuum pump is opened, control material thickness is 12mm；Setting pressure is
58Pa, temperature of heating plate is 48 DEG C, and drying time is 10.5h.
(3) distil for second：Control material thickness is 10mm；Setting pressure is 58Pa, and temperature of heating plate is 58 DEG C, constant temperature
1.6h is dried, material moisture is controlled within 5%.
(4) lose heart：Leakage pressure is set for 10Pa/min is lost heart.
(5) lose heart after terminating, continue the freeze-day with constant temperature 2.8h at 52 DEG C, freeze-drying process terminates.
Step 6, crushing：Crushed using micronizer, crossed 60 mesh sieves, obtained the homogeneous powdered stem of noble dendrobium of quality thin
Powder finished product.
Step 7, packaging：Nitrogen-filled packaging sealing is carried out in time to the stem of noble dendrobium freeze-dried powder after above-mentioned crushing, and is put in storage preservation.
Embodiment 3
A kind of preparation method of stem of noble dendrobium freeze-dried powder, comprises the following steps：
Step one, stem of noble dendrobium raw material are checked and accepted：HERBA DENDROBII originates from Xingyi City, Guizhou Province, the fresh stem of noble dendrobium.
Step 2, select and clean：Select without damaged without the stem of noble dendrobium for going mouldy, and remove blade；Then pure water rinsing stone is used
Dry measure used in former times.
Step 3, broken wall：Using super-pressure cryogenic technique, make stem of noble dendrobium cell membrane, cell membrane lysis, abundant release medicinal into
Divide and keep the activity of medicinal ingredient, can well protect the vivid color and luster of the stem of noble dendrobium.Super-pressure cryogenic technique treatment conditions are：Super
The cold water of the built-in certain volume of high-pressure bottle, container pressure is 500MPa, and pressurize 3min, temperature is 55 DEG C.
Step 4, defibrination are mixed：It is using fiberizer that the stem of noble dendrobium raw material after step 3 broken wall is levigate, it is less than stem of noble dendrobium granularity
10 μm, then mix.
Step 5, vacuum freeze drying：
(1) precooling：The outlet pressure of controlling pump is 0.08Mpa, opens compressor and plate low temperature valve, and control material thickness is
10mm；It is -38 DEG C to set precooling temperature, and the precooling time is 2.3h.
(2) distil for the first time：Plate low temperature valve is closed, vavuum pump is opened, control material thickness is 10mm；Setting pressure is
60Pa, temperature of heating plate is 45 DEG C, and drying time is 11h.
(3) distil for second：Control material thickness is 10mm；Setting pressure is 60Pa, and temperature of heating plate is 55 DEG C, constant temperature
1.8h is dried, material moisture is controlled within 5%.
(4) lose heart：Leakage pressure is set for 10Pa/min is lost heart.
(5) lose heart after terminating, continue the freeze-day with constant temperature 2.5h at 55 DEG C, freeze-drying process terminates.
Step 6, crushing：Crushed using micronizer, crossed 60 mesh sieves, obtained the homogeneous powdered stem of noble dendrobium of quality thin
Powder finished product.
Step 7, packaging：Nitrogen-filled packaging sealing is carried out in time to the stem of noble dendrobium freeze-dried powder after above-mentioned crushing, and is put in storage preservation.
Embodiment 4
A kind of preparation method of stem of noble dendrobium freeze-dried powder, comprises the following steps：
Step one, stem of noble dendrobium raw material are checked and accepted：Stem of Eyeshaped Dendrobium is called Dendrobium fimbriatum Hook, originates from City: A Case Study in Baise, the fresh stem of noble dendrobium.
Step 2, select and clean：Select without damaged without the stem of noble dendrobium for going mouldy, and remove blade；Then pure water rinsing stone is used
Dry measure used in former times.
Step 3, broken wall：Using super-pressure cryogenic technique, make stem of noble dendrobium cell membrane, cell membrane lysis, abundant release medicinal into
Divide and keep the activity of medicinal ingredient, can well protect the vivid color and luster of the stem of noble dendrobium.Super-pressure cryogenic technique treatment conditions are：Super
The cold water of the built-in certain volume of high-pressure bottle, container pressure is 520MPa, and pressurize 1min, temperature is 45 DEG C.
Step 4, defibrination are mixed：It is using fiberizer that the stem of noble dendrobium raw material after step 3 broken wall is levigate, it is less than stem of noble dendrobium granularity
10 μm, then mix.
Step 5, vacuum freeze drying：
(1) precooling：The outlet pressure of controlling pump is 0.09Mpa, opens compressor and plate low temperature valve, and control material thickness is
10mm；It is -39 DEG C to set precooling temperature, and the precooling time is 2.1h.
(2) distil for the first time：Plate low temperature valve is closed, vavuum pump is opened, control material thickness is 10mm；Setting pressure is
62Pa, temperature of heating plate is 42 DEG C, and drying time is 11.5h.
(3) distil for second：Control material thickness is 10mm；Setting pressure is 62Pa, and temperature of heating plate is 52 DEG C, constant temperature
1.9h is dried, material moisture is controlled within 5%.
(4) lose heart：Leakage pressure is set for 10Pa/min is lost heart.
(5) lose heart after terminating, continue the freeze-day with constant temperature 2.2h at 58 DEG C, freeze-drying process terminates.
Step 6, crushing：Crushed using micronizer, crossed 60 mesh sieves, obtained the homogeneous powdered stem of noble dendrobium of quality thin
Powder finished product.
Step 7, packaging：Nitrogen-filled packaging sealing is carried out in time to the stem of noble dendrobium freeze-dried powder after above-mentioned crushing, and is put in storage preservation.
Embodiment 5
A kind of preparation method of stem of noble dendrobium freeze-dried powder, comprises the following steps：
Step one, stem of noble dendrobium raw material are checked and accepted：Dendrobium thyrsiflorum originates from Yunnan Puer City, the fresh stem of noble dendrobium.
Step 2, select and clean：Select without damaged without the stem of noble dendrobium for going mouldy, and remove blade；Then pure water rinsing stone is used
Dry measure used in former times.
Step 3, broken wall：Using super-pressure cryogenic technique, make stem of noble dendrobium cell membrane, cell membrane lysis, abundant release medicinal into
Divide and keep the activity of medicinal ingredient, can well protect the vivid color and luster of the stem of noble dendrobium.Super-pressure cryogenic technique treatment conditions are：Super
The cold water of the built-in certain volume of high-pressure bottle, container pressure is 550MPa, and pressurize 2min, temperature is 40 DEG C.
Step 4, defibrination are mixed：It is using fiberizer that the stem of noble dendrobium raw material after step 3 broken wall is levigate, it is less than stem of noble dendrobium granularity
10 μm, then mix.
Step 5, vacuum freeze drying：
(1) precooling：The outlet pressure of controlling pump is 0.1Mpa, opens compressor and plate low temperature valve, control material thickness
10mm；It is -40 DEG C to set precooling temperature, and the precooling time is 2h.
(2) distil for the first time：Plate low temperature valve is closed, vavuum pump, control material thickness 10mm is opened；Setting pressure is 65Pa,
Temperature of heating plate is 40 DEG C, and drying time is 12h.
(3) distil for second：Control material thickness 10mm；Setting pressure is 65Pa, and temperature of heating plate is 50 DEG C, and constant temperature is done
Dry 2h, makes material moisture control within 5%.
(4) lose heart：Leakage pressure is set for 10Pa/min is lost heart.
(5) lose heart after terminating, continue the freeze-day with constant temperature 2h at 60 DEG C, freeze-drying process terminates.
Step 6, crushing：Crushed using micronizer, crossed 60 mesh sieves, obtained the homogeneous powdered stem of noble dendrobium of quality thin
Powder finished product.
Step 7, packaging：Nitrogen-filled packaging sealing is carried out in time to the stem of noble dendrobium freeze-dried powder after above-mentioned crushing, and is put in storage preservation.
Embodiment 6
In the present embodiment step one, stem of noble dendrobium raw material is checked and accepted and is：Dendrobium originates from Guangxi region, the fresh stem of noble dendrobium.Other are same
Embodiment 5.
Embodiment 7
In the present embodiment step one, stem of noble dendrobium raw material is checked and accepted and is：Dendrobium loddigesii Rolfe originates from Xingyi City, Guizhou Province, the fresh stem of noble dendrobium.Its
It is with embodiment 5.
Embodiment 8
In the present embodiment step one, stem of noble dendrobium raw material is checked and accepted and is：Purple dendrobium originates from Lijiang, yunnan city Huaping County, fresh stone
Dry measure used in former times.The other the same as in Example 5.
Comparative example 1
Do not include the broken wall of step 3, the other the same as in Example 5 in this example.
Comparative example 2
The vacuum freeze drying of step 5 is changed in this example dry in a conventional oven, the other the same as in Example 5.
The UV detection stems of noble dendrobium are respectively adopted to the stem of noble dendrobium freeze-dried powder that the embodiment of the present invention 1~8 and comparative example 1~2 are prepared
The content of polysaccharide, using the content and the content using cumarin in the HPLC detection stems of noble dendrobium of gas chromatography detection dendrobine.
The stem of noble dendrobium raw material that each group takes same batch is processed, the measurement result such as table 1 below of dendrobium polysaccharide content, stem of noble dendrobium alkali content
Measurement result such as table 2 below, cumarin content detection result such as table 3 below.
Table 1
Table 2
Table 3
It is lyophilized obtained by the preparation method of the embodiment of the present invention 1~8 compared with two comparative examples from the result of upper table 1
Powder, its polyoses content only reduces by 0.5% or so, does not almost lose；And the polyoses content reduction of two comparative examples is up to
More than 13.54%, polysaccharide loss degree is high.
It is lyophilized obtained by the preparation method of the embodiment of the present invention 1~8 compared with two comparative examples from the result of upper table 2
Powder, its alkali content only reduces by 1.63% or so, does not almost lose；And the alkali content reduction up to 20% of two comparative examples with
On, alkali loss degree is high.
It is lyophilized obtained by the preparation method of the embodiment of the present invention 1~8 compared with two comparative examples from the result of upper table 3
Powder, its tonka-bean cellulose content only reduces by 1.3% or so, does not almost lose；And the tonka-bean cellulose content reduction of two comparative examples is up to
More than 12.02%, the cumarin extent of damage is high.
The UV detections being related in the embodiment of the present invention use following detection method：According to《Chinese Pharmacopoeia》(2010 editions) first
The method of the lower polysaccharide specifications of assay is measured in portion's " dendrobium candidum ".
The vapor detection being related in the embodiment of the present invention uses following detection method：According to《Chinese Pharmacopoeia》(2010 editions)
The method that the lower HERBA DENDROBII of assay specifies in one " stem of noble dendrobium " is measured.
The HPLC detections being related in the embodiment of the present invention use following detection method：
Chromatographic condition：Chromatographic column is Sepax C18-H (250mm X 4.6mm, 5 μm), and mobile phase is methyl alcohol -1% formic acid
(25：75), flow velocity is 1ml/min, and Detection wavelength is 274nm, and column temperature is 30 DEG C.Theoretical cam curve presses the calculating of cumarin peak should not
Less than 5000.
The preparation of reference substance solution：Precision weighs cumarin reference substance in right amount, plus methyl alcohol is made every lml 58ug containing cumarin
Solution, obtain final product.
The preparation of test article solution：This product about 3g is taken, it is accurately weighed, to put in conical flask with cover, precision adds methyl alcohol 30ml,
Close plug, weighed weight ultrasonically treated 45 minutes, is let cool, then weighed weight, and the weight of less loss is supplied with methyl alcohol, is shaken up, filtration；
Subsequent filtrate is taken, is obtained final product.
Determination method：It is accurate respectively to draw reference substance solution and each 10ul of need testing solution, liquid chromatograph is injected, determine,
Obtain final product.
Applicant states that the present invention illustrates detailed process equipment of the invention and technological process by above-described embodiment,
But the invention is not limited in above-mentioned detailed process equipment and technological process, that is, do not mean that the present invention has to rely on above-mentioned detailed
Process equipment and technological process could be implemented.Person of ordinary skill in the field it will be clearly understood that any improvement in the present invention,
Addition, the selection of concrete mode to the equivalence replacement and auxiliary element of each raw material of product of the present invention etc., all fall within of the invention
Within the scope of protection domain and disclosure.
Claims (10)
1. a kind of preparation method of stem of noble dendrobium freeze-dried powder, it is characterised in that：Comprise the following steps：
Step one, broken wall is carried out to fresh stem of noble dendrobium raw material using super-pressure cryogenic technique；
Step 2, by the stem of noble dendrobium raw material after broken wall by defibrination mixing after, dendrobe powder is obtained using vacuum freeze drying；It is described true
Vacuum freecing-dry process is specifically included：Stem of noble dendrobium raw material after defibrination is mixed carries out precooling, for the first time distillation and second successively
Secondary distillation；
Step 3, dendrobe powder is carried out into ultramicro grinding treatment.
2. the preparation method of stem of noble dendrobium freeze-dried powder according to claim 1, it is characterised in that：The stem of noble dendrobium raw material is selected from copper sheet
One kind in the stem of noble dendrobium, Herba Dendrobii, HERBA DENDROBII, stem of Eyeshaped Dendrobium, Dendrobium thyrsiflorum, dendrobium, dendrobium loddigesii Rolfe and purple dendrobium.
3. the preparation method of stem of noble dendrobium freeze-dried powder according to claim 1, it is characterised in that：Also include before the step one
Select without damaged without the stem of noble dendrobium for going mouldy, and remove blade and cleaning.
4. the preparation method of stem of noble dendrobium freeze-dried powder according to claim 1, it is characterised in that：It is described super in the step one
High pressure low temperature technical conditions are specifically included：Pressure is 450~550MPa, 1~3min of pressurize；Temperature is 40~60 DEG C.
5. the preparation method of stem of noble dendrobium freeze-dried powder according to claim 1, it is characterised in that：In the step 2, the mill
Stem of noble dendrobium granularity is set to be less than 10 μm after slurry.
6. the preparation method of stem of noble dendrobium freeze-dried powder according to claim 1, it is characterised in that：It is described pre- in the step 2
The condition of freezing includes：The outlet pressure of the pump of vacuum freeze drier is set to 0.05~0.1Mpa；Control material thickness
It is 10~20mm, precooling temperature is -35 DEG C~-40 DEG C, and the precooling time is 2~2.5h.
7. the preparation method of stem of noble dendrobium freeze-dried powder according to claim 1, it is characterised in that：In the step 2, described
The condition for once distilling includes：Control material thickness is 10~20mm, and pressure is 55~65Pa, and drying temperature is 40~50 DEG C
When, drying time is 10~12h.
8. the preparation method of stem of noble dendrobium freeze-dried powder according to claim 1, it is characterised in that：In the step 2, described
The condition of secondary distillation includes：Control material thickness is 10~20mm, and 55~65Pa of pressure, drying temperature is 50~60 DEG C, is done
The dry time is 1.5~2h.
9. the preparation method of stem of noble dendrobium freeze-dried powder according to claim 1, it is characterised in that：In the step 2, described
Also include setting that leakage pressure, for 10~15Pa/min is lost heart, then proceedes to dry 2 at 50~60 DEG C after secondary distillation
~3h.
10. the preparation method of stem of noble dendrobium freeze-dried powder according to claim 1, it is characterised in that：In the step 3, by the stem of noble dendrobium
Powder also included 60 mesh sieves after carrying out ultramicro grinding.
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| CN111076504A (en) * | 2019-12-27 | 2020-04-28 | 通标标准技术服务（天津）有限公司 | Method for freeze-drying heat-sensitive substance |
| CN111426149A (en) * | 2020-03-27 | 2020-07-17 | 广西农业职业技术学院 | Dendrobium officinale freeze-drying method |
| CN111426149B (en) * | 2020-03-27 | 2022-05-24 | 广西农业职业技术大学 | Dendrobium officinale freeze-drying method |
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