CN103040877B - Preparation method of cordyceps sinensis micropowder lozenges - Google Patents
Preparation method of cordyceps sinensis micropowder lozenges Download PDFInfo
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Abstract
A preparation method of cordyceps sinensis micropowder lozenges relates to a technology that the cordyceps sinensis is smashed through an ultra-low temperature smashing method and then is frozen and dried to produce the cordyceps sinensis micropowder which serves as the raw material, and then the raw material is rehydrated and pressed to obtain the cordyceps sinensis micropowder lozenges. The method comprises the following steps: first: freezing the cordyceps sinensis with water content not less than 5 percent to be below 0 DEG C, and smashing under the temperature not higher than 0 DEG C; directly freezing and drying the non-defrosting cordyceps sinensis micropowder obtained through smashing, wherein the water content of the micro powder at the moment is not higher than 3 percent (weight); forwards, rehydrating the frozen and dried cordyceps sinensis micropowder; allowing the water for rehydration to be subjected to ultrasonic atomization so as to obtain water mist which is input into the frozen and dried micro powder; meanwhile, stirring the frozen and dried micro powder so as to allow the water content to be raised to 4-20 percent (weight), and obtaining the rehydrated micro powder with the water percent of 4-20 percent (weight); and tabletting the micro powder so as to obtain the cordyceps sinensis micropowder lozenges with the water content not high than 20 percent (weight). The cordyceps sinensis micropowder with water content lower than 8 percent can be directly pressed into the lozenges with uniform water content, and the method for controlling the water content is simple and precise.
Description
Technical field
The aweto micropowder that the present invention relates to obtain after the pulverizing of pulverizing at ultralow temperature method, lyophilization using Cordyceps is as raw material, and rehydration tabletting is prepared a kind of technology of aweto micropowder low water content buccal tablet.Belong to the scope of medicine, food and health product.
Background technology
Cordyceps
(Cordyceps sinensis)the traditional precious Chinese medicine of China, in the use history of state-owned more than one thousand years.Modern medicine study shows, Cordyceps has the multiple efficacies such as the function of immune system of adjusting, antitumor, resisting fatigue.Effective ingredient wherein for example contains the polysaccharide of protein subunit, and has various albumen and the enzyme of anticancer, antitumor and startup immunocompetence, under the condition of too high temperature, all can be hydrolyzed and destroy.This just makes tradition utilize the mode inefficiency of Cordyceps.In Chinese patent ZL200810303308.8, propose first the pressing process of the pure powder sheet of Cordyceps, wherein main innovate point is the pure micropowder of Cordyceps under the moisture between 8 ~ 18%, to carry out tabletting, and once or repeatedly compacting is in blocks.The micropowder tablet pressing process of actual water content between 9 ~ 12%.Micropowder thickness very easily after directly adding water, is difficult to be mixed evenly, and while using the method, micropowder water content can not be suppressed in flakes lower than 8%.In the patent application that is 201210128486.8 at application number, disclose and a kind ofly first water content is prepared into nano powder lower than 9% Cordyceps, then nano powder is added weight to be prepared into homogenate in the water of 2 ~ 6 times, to after homogenate lyophilizing, again pulverize again, mixed former nano powder carries out tabletting, due in the work process of freeze dryer, be difficult to direct sample and carry out determination of water, can not accurately control the water content of material by freeze-dry process, have to add former nano powder to regulate water content in lyophilized powder, it is higher that this just makes accurately to control before tabletting the water content difficulty of material.Be lyophilized in the process of medicated powder at homogenate, because add water, after homogenate, the stickum in Cordyceps cell is dissolved in water in a large number, in freeze-drying process, material layering in homogenate in freezing process, the uneven components of the lump material after lyophilizing, surface becomes the black color of unbuttoning or divest one's upper garment, and inside is Lycoperdon polymorphum Vitt, need again pulverize and just can obtain the uniform micropowder of comparison of ingredients, make production technology become complicated.
summary of the invention:
the invention provides a kind of preparation method of low moisture aweto micropowder buccal tablet, first under the temperature environment below 0 ℃, Cordyceps is pulverized, then the aweto micropowder after pulverizing is directly carried out to lyophilizing, again aweto micropowder after lyophilizing is adopted ultrasonic atomizatio mode that water content is pressed into buccal tablet after lower than 3% freeze-dry micropowder rehydration, water content and the composition of the buccal tablet making are even, and the control method of buccal tablet water content is simple and accurate.
A preparation method for aweto micropowder buccal tablet, comprises the following steps:
First, get water content be not less than 5% Cordyceps be chilled to 0 ℃ following and pulverize under not higher than the environment of 0 ℃, will pulverize the direct lyophilizing of aweto micropowder of gained, the Cordyceps freeze-dry micropowder water content after lyophilizing is not higher than 3%(weight);
Then, by Cordyceps freeze-dry micropowder rehydration: water ultrasonic atomizatio used rehydration is become in water smoke input freeze-dry micropowder, stir freeze-dry micropowder and make its water content evenly be elevated to 4 ~ 20%(weight simultaneously), obtaining water content is 4 ~ 20%(weight) rehydration micropowder;
By gained rehydration micropowder tabletting, obtain the pure powder buccal tablet of Cordyceps again.
onthe preparation method of a kind of aweto micropowder buccal tablet of stating, described by Cordyceps freeze-dry micropowder rehydration, makes its water content evenly be elevated to 4 ~ 7.9%(weight), obtaining water content is 4 ~ 7.9%(weight) rehydration micropowder.
onthe preparation method of a kind of aweto micropowder buccal tablet of stating, the amount of described rehydration water used, refers to and first calculates according to the water content meter of the rehydration micropowder after the water content of freeze-dry micropowder before rehydration, quality and rehydration the water yield that needs ultrasonic atomizatio.
onthe preparation method of a kind of aweto micropowder buccal tablet of stating, the Cordyceps water content before described pulverizing is not less than 10%(weight).
onthe preparation method of a kind of aweto micropowder buccal tablet of stating, the Cordyceps before described pulverizing is fresh Cordyceps.
The preparation method of above-mentioned a kind of aweto micropowder buccal tablet, the Cordyceps before described pulverizing is the fresh Cordyceps after dehydration in the low temperature environment below 25 ℃.
onthe preparation method of a kind of aweto micropowder buccal tablet of stating, the aweto micropowder of described pulverizing gained refers to the micropowder of diameter between 0.02 ~ 50 μ m.
onthe preparation method of a kind of aweto micropowder buccal tablet of stating, the water content of described rehydration micropowder is 5-7.9%(weight).
onthe preparation method of a kind of aweto micropowder buccal tablet of stating, the water content of described rehydration micropowder is 7%(weight).
onthe preparation method of a kind of aweto micropowder buccal tablet of stating, described pulverizing is carried out in protective atmosphere.
Beneficial effect:
The way of taking directly complete lyophilizing, makes the moisture in its lyophilized powder directly drop to lyophilizing terminal, then calculates by the water content of rehydration micropowder after micropowder weight, water content and rehydration before rehydration the moisture weight that needs interpolation; By ultrasound wave by the moisture atomization calculating, by even micropowder moistening rehydration; Make rehydration micropowder water content precisely controlled, because the hydrone after atomization has changed the surface nature of micropowder, and on micropowder basis after this moistening, directly carry out tabletting easy operating, buccal tablet tabletting rate is high, the novel powder buccal tablet of Cordyceps obtaining, effectively preserving under the prerequisite that effective ingredient do not lose, has water content low, constant product quality, the advantages such as tablet outward appearance is good, and disintegration rate is fast, and effective ingredient stripping is fast.Under condition of ultralow temperature, prepare aweto micropowder and superfine powder, do not add any adjuvant, micropowder and superfine powder are carried out to lyophilizing and obtain its lyophilized powder, its original effective ingredient can all be retained.
the amount of rehydration water usedrefer to and first calculate according to the water content meter of the water content of freeze-dry micropowder, quality, rehydration micropowder the water yield that needs ultrasonic atomizatio, before rehydration, just rehydration amount is decided, only needed ultrasonic atomizatio to determine that the water of weight just can control the water content of rehydration micropowder, can realize the water content homogeneous of buccal tablet.
Owing to not adding any antiseptic or other material in the pure powder buccal tablet of Cordyceps, if the words that levels is too high, in pharmacopeia, require at present the adenosine and the cordycepin that detect to affect little, but to not detected by force at present, have impact but be proved to be important effective ingredient as the polysaccharide that contains protein subunit and enzyme, these effective ingredient can decompose in high moisture environments.Too high moisture also causes buccal tablet surface color excessively dark, by initial light brown and Lycoperdon polymorphum Vitt, becomes dark brown and pitchy.Affect buccal tablet presentation quality, be also unfavorable for the long-term reservation of effective ingredient simultaneously, the water content of the buccal tablet that the method for the invention is produced is during higher than 7.9% (weight), buccal tablet invariant color, and be conducive to long-term preservation.
Through lyophilizing aweto micropowder later, the existing part stripping of polysaccharide material wherein, on micropowder surface, is now carried out moistening to micropowder, and the hole between micropowder and micropowder reduces, and bonding force increases.Changed its poor fluidity, quality is light, and the feature that is easy to fly away has increased plasticity and mobility greatly.Because a small amount of stripping of polysaccharide becomes the binding agent between its natural micropowder, make the pure powder buccal tablet of Cordyceps that obtains low moisture (lower than 8%) become technically possibility simultaneously.And due to simple to operate, reliability is high, and tablet is of good quality, retain the micropowder character after lyophilizing, effective ingredient dissolution efficiency is also improved.
Demonstration test: get 100g Cordyceps 0.02 ~ 50 μ m micropowder, add 500g sterilized water to mix thoroughly, stirring and dissolving 60 minutes at 4 ℃, fully extract solable matter wherein, then centrifugal 20 minutes of 12000rpm, get after the lyophilizing in 8 hours of supernatant solution, obtain water content at 7% dark brown material 32g, this material viscosity is strong, detect through chromatograph and SDS-PAGE, wherein main component is various soluble polysaccharides and protein, getting this stickum of 25g fully mixes water content and carries out tabletting at 7% Cordyceps 0.02 ~ 50 μ m micropowder 45g, obtain water content at 7% Cordyceps buccal tablet, original pure aweto micropowder that cannot direct compression under low wash water, under the stickum of the own stripping of its Cordyceps bonding, can be pressed in flakes, this has illustrated, control the stripping of stickum, become the key factor of tabletting.
Due to lyophilizing effect, a small amount of polysaccharide and stickum can be at freeze-dry micropowder surface aggregations, and hydrone by atomization after, touch micropowder surface, the surface nature of micropowder is changed, and make surface viscosity material micro dissolution, after originally dry stickum micro dissolution, the surface viscosity of micropowder increases.Originally be difficult to disposable tabletting, need the micropowder of high pressure and high-moisture, can under relatively low pressure and low moisture condition, be pressed into buccal tablet.
The tablet forming technique difficult point of the pure powder buccal tablet of Cordyceps is how under the prerequisite of not adding any adjuvant, to carry out tabletting.Its key problem is the character that how to change micropowder, the aweto micropowder water content of just having pulverized is because technique is unusual between 5 ~ 15%, because moisture great majority now exist micropowder inside, due to the technique through broken, its micropowder surface nature is comparatively dried, the stickum great majority that it contains are also in the inner not release of micropowder, this just makes micropowder character light, dry Workflow, between micropowder, stress is also larger, now carry out the adjustment of moisture, its root problem still makes its internal viscosity material slightly soluble go out, micropowder surface nature is changed, thereby make the micropowder can direct compression.And the common technique that adds water stirs for being directly in harmonious proportion to intake in micropowder, because micropowder water absorption is extremely strong, this just causes the local moisture adding water high, need higher moisture (9.5%), just can make the even stripping of stickum in micropowder, the effect that micropowder surface nature changes.
And first we take the aweto micropowder of just having pulverized to carry out the technique of a step lyophilizing, make micropowder internal moisture in sublimation process, make micropowder surface there is spongiform structure, and in freeze-drying process, due to the distillation of moisture, stickum stripping is to micropowder surface, as now carried out the technique of ultrasound wave moistening, ultrasound wave can produce the particle water that micro-atomization is 1 ~ 5 μ m, the technique directly tempering than tradition, more can make uniformly micropowder moistening, and the surface of the aweto micropowder of lyophilizing is spongy, can strengthen this wetting effect, allow stickum stripping in micropowder, make micropowder there is viscosity, thereby stress between its micropowder is reduced, micropowder plasticity increases greatly, this becomes the key of low water content tabletting.
Through evidence: even do not become bulk but micropowder after water content, up to 70% fresh Cordyceps, is pulverized direct lyophilizing under not higher than the environment of 0 ℃.But micropowder becomes bulk at 0 ℃ after adding water above homogenate lyophilizing.First this and traditional handicraft are dried to moisture by Cordyceps under 60 ℃ of conditions increases fragility below 10%, then more than 0 ℃, room temperature is pulverized, and is essentially different.Under ultralow temperature, water content can be exceeded to 50% fresh Cordyceps and carry out one fast-crushing.And the quantity of reactive protein in fresh Cordyceps is far away higher than the dried Cordyceps of traditional handicraft.Due to freezing effect, in Cordyceps, hydrone becomes ice crystal, after pulverizing, becomes tiny granule together with aweto micropowder.The low temperature that keeps micropowder, does not thaw, and directly carries out lyophilizing program, obtains freeze-dry micropowder and can retain whole compositions, is also beneficial to the rehydration tabletting that carries out next step.And in traditional disintegrating process, in the application number patent application that is 201210128486.8, be moisture can not be carried out to one pulverizing higher than 9% Cordyceps.And in our technique, when Cordyceps is pulverized, moisture on the contrary can not be lower than 7%, otherwise stickum overflows the very few later stage tabletting that affects.This is cryogenic conditions wherein, has play a part important.Not only make the fresh herb can one fast-crushing at short notice, and the original effective ingredient that can retain its fresh Cordyceps destroy.And tradition is pulverized the grinding time that reaches 3 ~ 10 hours relatively, and grinding time of the present invention is generally no more than 2 hours.Consuming timely also obtain minimizing.
specific embodiments:
Embodiment 1
A low moisture buccal tablet processing technology for Cordyceps, its flow process comprises what the following steps were carried out: the preparation of micropowder, the preparation of lyophilized powder, the rehydration of lyophilized powder, tabletting, products measure.
The preparation of micropowder: get water content and be 10% Cordyceps 200g; under 0 ℃ of condition, pulverize; in crushing process; adopt the mode of liquid nitrogen refrigerating to carry out; the nitrogen of liquid nitrogen or liquid nitrogen volatilization contributes to prevent that Cordyceps from contacting and being oxidized with oxygen in pulverizing, the not oxidized inefficacy of protection effective ingredient.By ball mill or other crumbling method, at this temperature, Cordyceps is pulverized to 0.02 ~ 50 μ m, after having pulverized, micropowder is taken out for subsequent use.
The preparation of lyophilized powder: the aweto micropowder after above-mentioned steps is pulverized, diameter is between 0.02 ~ 50 μ m, color is light brown, the aweto micropowder crushing is put into freeze dryer, directly carry out lyophilizing program, control omnidistance temperature not higher than 35 ℃, after the freeze-drying process of 10h, micropowder moisture 2%, color is Lycoperdon polymorphum Vitt, takes out for subsequent use.
The rehydration of lyophilized powder: get water content and be 2% Cordyceps freeze-dry micropowder 100g, making the micropowder water content after rehydration is 5%, the rehydration amount that calculates demand is 3.2g, the sterilized water 3.2g of needs is put into soniclizer, open nebulizer, now moisture enters in Cordyceps freeze-dry micropowder in the mode of mist droplet, keep the low temperature of lyophilized powder, stir, make its moistening even, atomization 5 minutes, 3.2g water all enters in freeze-dry micropowder, stir again 20 minutes to obtain the uniform rehydration micropowder of water content, the water content of rehydration micropowder is 5% [rehydration amount computational methods: method one, moisture 2g in the Cordyceps freeze-dry micropowder 100g of rehydration front 2%, Y/(100-2+Y)=5%, Y=5.16 solves an equation to obtain, 5.16-2=3.16, method two, establish moisture Y gram in the rehydration micropowder after rehydration, obtain an equation, moisture 2g in the Cordyceps freeze-dry micropowder 100g of rehydration front 2%, after X gram, make the water content of 2% Cordyceps freeze-dry micropowder 100g become 5% if need add water, obtain an equation: (X+2)/(X+100)=5%, solve an equation to such an extent that X=3.16 is 3.2].
Tabletting: be that 5% rehydration micropowder directly carries out tablet forming technique by water content.According to varying in size and the weight specification of tablet of micropowder, to optimize its pressure and moisture ratio, as take micropowder diameter at 5 ~ 15 μ m, water content is at 5% pure powder tabletting, and hardness is in 4.5kg left and right.
Detect: obtain the Cordyceps low wash water buccal tablet of different size, according to pharmacopeia and relevant criterion flow process, measure adenosine, the step of the compositions such as cordycepin.Product after qualified, encapsulates and sells.
In embodiment 1, when pulverizing, getting water content is 4%, 5%, 7%, 7.9%, 8%, 10%, 15%, Cordyceps, repeat after above-mentioned steps to find: the Cordyceps water content before pulverizing lower than 7% time, rate in blocks low (85%) when tabletting, analysis be because of moisture in micropowder before lyophilizing very little, when lyophilizing, overflow goo reduce; Cordyceps water content before pulverizing is 8%, 10%, 15% time, overflows goo more when lyophilizing, rate in blocks high (85 ~ 95%) when tabletting, and the Cordyceps water content before pulverizing is between 10% or 15% time, in flakes rate the highest (95%).
In embodiment 1, protective gas, except nitrogen, also can be selected the gas such as helium, carbon dioxide.
Embodiment 2
The preparation of micropowder: the clean Cordyceps of choosing after sterilization and sterilizing carries out low temperature moisture pump, obtains moisture and is 15% Cordyceps.Cordyceps is put into special pulverizer and pulverize, add liquid nitrogen, temperature is controlled at-196 ℃, pulverizes 30min, and now aweto micropowder diameter is between 5 ~ 15 μ m.Now aweto micropowder color is filbert to Lycoperdon polymorphum Vitt.
The preparation of lyophilized powder: by being crushed to the aweto micropowder of fineness, put into freeze dryer, enter lyophilizing program, freeze-drying process temperature is no more than 35 ℃, lyophilizing program 8h, moisture 2%, now Cordyceps freeze-dry micropowder color is canescence.
The rehydration of lyophilized powder: take diameter 5 ~ 15 μ m, the Cordyceps freeze-dry micropowder 1000g of moisture 2%.Cordyceps freeze-dry micropowder is put into 4 ℃ of environment; calculate water requirement 32g; sterilized water is carried out to micronize by ultrasonic atomization machine; water microgranule imports in Cordyceps freeze-dry micropowder by flexible pipe, in this process, Cordyceps freeze-dry micropowder is stirred, and makes its even moistening; this process is at 30min; adjusting final moisture amount is 5%, and after Chinese caterpillar fungus freeze-dried powder rehydration, appearance color is Lycoperdon polymorphum Vitt.
Tabletting: carry out tabletting take every of 0.25g as specification, adjust pressure, one-shot forming rate is 95%, and hardness 4.5kg, obtains 3920 of every tablet of specification buccal tablets of 0.25g.
Detect: with reference to extremely relevant criterion of pharmacopeia, in chromatograph mode to wherein determining adenosine, the step of the compositions such as cordycepin.Product after qualified, encapsulates and sells.
In embodiment 2, when when rehydration, the weight of atomized water is 195.12g, the water content of rehydration micropowder is 18%; When rehydration, the weight of atomized water is 153g, the water content of rehydration micropowder is 15%; When rehydration, the weight of atomized water is 88g, the water content of rehydration micropowder is 10%; When rehydration, the weight of atomized water is 65g, the water content of rehydration micropowder is 8%; When rehydration, the weight of atomized water is 53g, the water content of rehydration micropowder is 7%.
Embodiment 3
The preparation of micropowder: the clean Cordyceps of choosing after sterilization and sterilizing carries out moisture pump, moisture 5%.The Cordyceps herb of this content is put into special pulverizer and pulverize, add liquid nitrogen, temperature is controlled at-196 ℃, pulverizes 200min, and now aweto micropowder diameter is between 0.5 ~ 0.8 μ m.Now aweto micropowder color is filbert to Lycoperdon polymorphum Vitt.
The preparation of lyophilized powder: by being crushed to the aweto micropowder of fineness, put into freeze dryer, enter lyophilizing program, freeze-drying process temperature is no more than 35 ℃, lyophilizing program 12h, moisture 1.2%, now Cordyceps freeze-dry micropowder color is canescence.
The rehydration of lyophilized powder: take diameter 0.5 ~ 0.8 μ m, the Cordyceps freeze-dry micropowder 1000g of moisture 1.2%.Cordyceps freeze-dry micropowder is put into 4 ℃ of environment; calculate water requirement 63g, sterilized water is carried out to micronize by ultrasonic atomization machine, water microgranule imports in Cordyceps freeze-dry micropowder by flexible pipe; in this process, Cordyceps freeze-dry micropowder is carried out to micro-stirring, make its even moistening.This process is at 40min.Adjusting final moisture amount is 7%, and after Chinese caterpillar fungus freeze-dried powder rehydration, appearance color is Lycoperdon polymorphum Vitt.
Tabletting: carry out tabletting take every of 0.25g as specification, adjust pressure, one-shot forming rate is 85%, and hardness 4.1kg, obtains 3398 of every tablet of specification buccal tablets of 0.25g.
Detect: with reference to extremely relevant criterion of pharmacopeia, in chromatograph mode to wherein determining adenosine, the step of the compositions such as cordycepin.Product after qualified, encapsulates and sells.
Embodiment 4
The preparation of micropowder: the clean Cordyceps of choosing after sterilization and sterilizing carries out moisture pump, moisture 15%.The Cordyceps herb of this content is put into special pulverizer and pulverize, add liquid nitrogen, temperature is controlled at-196 ℃, pulverizes 100min, and now aweto micropowder diameter is between 0.5 ~ 0.8 μ m.Now aweto micropowder color is filbert to Lycoperdon polymorphum Vitt.
The preparation of lyophilized powder: by being crushed to the aweto micropowder of fineness, put into freeze dryer, enter lyophilizing program, freeze-drying process temperature is no more than 35 ℃, and lyophilizing program 12h, obtains freeze-dry micropowder moisture 3%, and now Cordyceps freeze-dry micropowder color is canescence.
The rehydration of lyophilized powder: take diameter 0.5 ~ 0.8 μ m, the Cordyceps freeze-dry micropowder 1000g of moisture 3%.Cordyceps freeze-dry micropowder is put into 4 ℃ of environment; calculate water requirement 43g, sterilized water is carried out to micronize by ultrasonic atomization machine, water microgranule imports in Cordyceps freeze-dry micropowder by flexible pipe; in this process, Cordyceps freeze-dry micropowder is carried out to micro-stirring, make its even moistening.This process is at 40min.Adjusting final moisture amount is 7%, and after Chinese caterpillar fungus freeze-dried powder rehydration, appearance color is Lycoperdon polymorphum Vitt.
Tabletting: carry out tabletting take every of 0.25g as specification, adjust pressure, one-shot forming rate is 85%, and hardness 4.1kg, obtains 3398 of every tablet of specification buccal tablets of 0.25g.
Detect: with reference to extremely relevant criterion of pharmacopeia, in chromatograph mode to wherein determining adenosine, the step of the compositions such as cordycepin.Product after qualified, encapsulates and sells.
Embodiment 5
The preparation of micropowder: choose the fresh Cordyceps of cleaning after sterilization and sterilizing, moisture 70%.The Cordyceps herb of this content is put into special pulverizer and pulverize, add liquid nitrogen, temperature is controlled at-196 ℃, pulverizes 100min, and now aweto micropowder diameter is between 0.5 ~ 0.8 μ m.Now aweto micropowder color is filbert to Lycoperdon polymorphum Vitt.
The preparation of lyophilized powder: will be crushed to the aweto micropowder of fineness, temperature is-20 ℃ does not thaw, and puts into freeze dryer, enters lyophilizing program, and freeze-dry micropowder moisture is dropped to below 3%, and now Cordyceps freeze-dry micropowder color is canescence.
The rehydration of lyophilized powder: take diameter 0.5 ~ 0.8 μ m, the Cordyceps freeze-dry micropowder 1000g of moisture 3%.Cordyceps freeze-dry micropowder is put into 4 ℃ of environment; calculate water requirement 43g, sterilized water is carried out to micronize by ultrasonic atomization machine, water microgranule imports in Cordyceps freeze-dry micropowder by flexible pipe; in this process, Cordyceps freeze-dry micropowder is carried out to micro-stirring, make its even moistening.This process is at 40min.Adjusting final moisture amount is 7%, and after Chinese caterpillar fungus freeze-dried powder rehydration, appearance color is Lycoperdon polymorphum Vitt.
Tabletting: carry out tabletting take every of 0.25g as specification, adjust pressure, one-shot forming rate is 85%, and hardness 4.1kg, obtains 3398 of every tablet of specification buccal tablets of 0.25g.
In above-described embodiment, can adopt following method to prepare Chinese caterpillar fungus freeze-dried powder: comprise the pure micropowder of Cordyceps or superfine powder are carried out to prefreezing, primary drying, the steps such as parsing-desiccation:
A, prefreezing: freezing 0.1 ~ 2h under the condition of 0 ~-150 ℃ by the pure micropowder of the Cordyceps having prepared or superfine powder;
B, primary drying: the pure micropowder of the Cordyceps after prefreezing or superfine powder under lower than 50pa condition, cascade raising temperature to 30 ℃, this primary drying process is at 1 ~ 10h;
C, parsing-desiccation: the pure micropowder of the Cordyceps after primary drying or superfine powder are placed in to the not temperature higher than 35 ℃, and air pressure under the condition higher than 15pa, was not drained residual moisture in 1 ~ 10 hour, and lyophilized powder moisture content of finished products content drops to 0.01 ~ 10%.
Embodiment 6
The preparation of micropowder: choose the fresh Cordyceps of cleaning after sterilization and sterilizing, moisture 70%.The Cordyceps herb of this water content is put into special pulverizer and pulverize, add liquid nitrogen, temperature is controlled at-196 ℃, pulverizes 100min, and now aweto micropowder diameter is between 0.5 ~ 0.8 μ m, and now aweto micropowder color is filbert to Lycoperdon polymorphum Vitt.
The preparation of lyophilized powder: by being crushed to the aweto micropowder of fineness, put into freeze dryer, enter lyophilizing program, freeze-dry micropowder moisture is dropped to below 3%, now Cordyceps freeze-dry micropowder color is canescence.
The rehydration of lyophilized powder: take diameter 0.5 ~ 0.8 μ m; the Cordyceps freeze-dry micropowder 1000g of moisture 1%; Cordyceps freeze-dry micropowder is put into 4 ℃ of environment; calculate water requirement 75g; sterilized water is carried out to micronize by ultrasonic atomization machine; water microgranule imports in Cordyceps freeze-dry micropowder by flexible pipe, in this process, Cordyceps freeze-dry micropowder is stirred, and makes its even moistening.This process is at 40min.Adjusting final moisture content is 7.9%, and after Chinese caterpillar fungus freeze-dried powder rehydration, appearance color is Lycoperdon polymorphum Vitt.
Tabletting: carry out tabletting take every of 0.25g as specification, adjust pressure, one-shot forming rate is 82%, and hardness 4.3kg, obtains 3526 of every tablet of specification buccal tablets of 0.25g.
Embodiment 7
The preparation of micropowder: choose the fresh Cordyceps of cleaning after sterilization and sterilizing, moisture 70%.The Cordyceps herb of this moisture is put into special pulverizer and pulverize, add liquid nitrogen, temperature is controlled at-196 ℃, pulverizes 100min, and now aweto micropowder diameter is between 0.5 ~ 0.8 μ m.Now aweto micropowder color is filbert to Lycoperdon polymorphum Vitt.
The preparation of lyophilized powder: by being crushed to the aweto micropowder of fineness, put into freeze dryer, enter lyophilizing program, freeze-dry micropowder moisture is dropped to below 3%, now Cordyceps freeze-dry micropowder color is canescence.
The rehydration of lyophilized powder: take diameter 0.5 ~ 0.8 μ m, the Cordyceps freeze-dry micropowder 1000g of moisture 0.7%.Cordyceps freeze-dry micropowder is put into 4 ℃ of environment; calculate water requirement 34g, sterilized water is carried out to micronize by ultrasonic atomization machine, water microgranule imports in Cordyceps freeze-dry micropowder by flexible pipe; in this process, Cordyceps freeze-dry micropowder is stirred, make its even moistening.This process is at 40min.Adjusting final moisture amount is 4%, and after Chinese caterpillar fungus freeze-dried powder rehydration, appearance color is canescence.
Tabletting: carry out tabletting take every of 0.25g as specification, adjust pressure, one-shot forming rate is 76%, and hardness 4.4kg, obtains 3145 of every tablet of specification buccal tablets of 0.25g.
At the fresh Cordyceps described in embodiment 7, take off part moisture in can the low temperature environment below 25 ℃ and pulverize again.
Embodiment 8
The preparation of micropowder: choose the fresh Cordyceps of cleaning after sterilization and sterilizing, moisture 70%.The Cordyceps herb of this moisture is put into special pulverizer and pulverize, add liquid nitrogen, temperature is controlled at-196 ℃, pulverizes 100min, and now aweto micropowder diameter is between 0.5 ~ 0.8 μ m.Now aweto micropowder color is filbert to Lycoperdon polymorphum Vitt.
The preparation of lyophilized powder: by being crushed to the aweto micropowder of fineness, put into freeze dryer, enter lyophilizing program, freeze-dry micropowder moisture is dropped to below 3%, now Cordyceps freeze-dry micropowder color is canescence.
The rehydration of lyophilized powder: take diameter 0.5 ~ 0.8 μ m, the Cordyceps freeze-dry micropowder 1000g of moisture 2%.Cordyceps freeze-dry micropowder is put into 4 ℃ of environment; calculate water requirement 225g, sterilized water is carried out to micronize by ultrasonic atomization machine, water microgranule imports in Cordyceps freeze-dry micropowder by flexible pipe; in this process, Cordyceps freeze-dry micropowder is stirred, make its even moistening.This process is at 60min.Adjusting final moisture amount is 20%, after the Chinese caterpillar fungus freeze-dried powder rehydration of this water content, and appearance color pitchy.
Tabletting: carry out tabletting take every of 0.25g as specification, adjust pressure, one-shot forming rate is 52%, and hardness 2.3kg, obtains 2500 of every tablet of specification buccal tablets of 0.25g.Because moisture is too high, cause sticking phenomenon, tabletting rate is low, and tablet quality is bad.
In above-described embodiment, can adopt following method to prepare Chinese caterpillar fungus freeze-dried powder: comprise the pure micropowder of Cordyceps or superfine powder are carried out to prefreezing, primary drying, the steps such as parsing-desiccation:
A, prefreezing: freezing 0.1 ~ 2h under the condition of 0 ~-150 ℃ by the pure micropowder of the Cordyceps having prepared or superfine powder;
B, primary drying: the pure micropowder of the Cordyceps after prefreezing or superfine powder under lower than 50pa condition, cascade raising temperature to 30 ℃, this primary drying process is at 1 ~ 10h;
C, parsing-desiccation: the pure micropowder of the Cordyceps after primary drying or superfine powder are placed in to the not temperature higher than 35 ℃, and air pressure under the condition higher than 15pa, was not drained residual moisture in 1 ~ 10 hour, and lyophilized powder moisture content of finished products content drops to 0.01 ~ 10%.
Because vacuum lyophilization is dewatered under low temperature, low pressure, and moisture directly distils, Vacuum Freezing & Drying Technology makes the heat sensitive material in pure micropowder or the superfine powder of Cordyceps also can dewater more thorough, and the pure micropowder of the Cordyceps of drying or superfine powder are stable, are convenient to long time stored; Because being dried under frozen state of material completes, compared with other drying means, physical arrangement and the molecule structure change of material are minimum, and beneficiating ingredient is not damaged; In vacuum lyophilization process, there is not surperficial sclerosis problem in material, and it inner forms the spongy of porous, thereby have excellent rehydration, and the pure micropowder of Cordyceps or superfine powder can absorb water at short notice, and its benefit materials can be soluble in water fast; Because the phorozoon of Cordyceps is fungus China pilose spore, this bacterium natural distributed is more than 3000 meters plateaus in height above sea level, for having a liking for cold low temperature fungus.This bacterium just can not grow at 25 ℃, and 30 ℃ will be destroyed by high temperature because of physiological function and death.Because dry run is to carry out at low temperatures, and substantially completely cut off air, therefore effectively suppressed heat-sensitive substance biology, chemistry or physical change have occurred, and preserve preferably the active substance in raw material, in cryodesiccated process, temperature is controlled at and is no more than 35 ℃, can wherein effective active composition of complete reservation.
required in above-described embodimentthe pure micropowder of Cordyceps or superfine powder: pure micropowder diameter is between 40 ~ 2000 orders, and superfine powder diameter is at 0.02 ~ 15 micron.Optional standby in order to below legal system: first Cordyceps to be chilled to below 0 ℃, then under not higher than the condition of 0 ℃ of degree, the Cordyceps being chilled to below 0 ℃ to be pulverized.
While adopting said method, preferably pulverized freezing Cordyceps is herb.
Be crushed to 40 ~ 2000 object products and be called pure micropowder.
The product that is crushed to 0.02 ~ 15 micron is called superfine powder.
In the present invention, the pure micropowder of Cordyceps used or superfine powder, preferably the fresh Cordyceps after cleaning and sterilization treatment is processed and obtains through said method.
While pulverizing lyophilizing in above-described embodiment, vacuum available pump suction air, reduces or control air pressure.
In above-described embodiment, when tabletting, optimum pressure is 45KN.
In above-described embodiment, the computational methods of rehydration amount are: first calculate after rehydration moisture quality a in gained rehydration micropowder, then calculate the quality b of the water in freeze-dry micropowder before rehydration, a-b is exactly atomization rehydration amount.
In prior art, Cordyceps need to first be dried and pulverize, and its moisture is no more than 10% in order to increase its fragility, could be ground into micropowder by ball mill etc.The too high Cordyceps of water quantities can not be ground into micropowder because toughness is too high.But through research (Jin Chaoxia. the protein science preliminary study .2005. Nankai University of Cordyceps): dry the Cordyceps of placing after a period of time and carry out 2D-E (two dimensional gel electrophore-sis) and analyze, can only detect 18 kinds of protein, and the contained protein quantity of Cordyceps under fresh state, by analyzing, be not less than 10000 kinds of protein.Analyze from protein science meaning, room temperature is pulverized after drying again, and wherein the loss of protein quantity may be up to more than 99%.In pharmacopeia, only require adenosine and cordycepin content to Cordyceps to carry out compulsory test at present, and prove that through modern pharmacology medicineization cancerous cell is had to the composition of lethal effect, as the polysaccharide that contains protein subunit, and various reactive protein does not do requirement.And reactive protein and most of polysaccharide are degraded to lose efficacy at too high temperature.When this is also modern pharmacology checking Cordyceps effect, take more 4 ℃ even lower temperature water extract verify the basic reason to various cancerous cell lethal effects.In the above-described embodiments, first take, under ultralow temperature, Cordyceps is carried out to freezing processing, increased the fragility of Cordyceps.Even if moisture also can be crushed to Nano grade up to 70% fresh Cordyceps under ultralow temperature.Its protein and other compositions can both be retained completely, and directly carry out freeze-dry process at the aweto micropowder that puts before this acquisition.Then by lyophilized powder rehydration tabletting, can really retain its whole compositions, again can be accurate and simple in moisture Control.And reduce the content of moisture in Cordyceps buccal tablet, be also beneficial to the long-term reservation of later stage effective ingredient.
Choosing in the above-described embodiments the different Cordyceps of water content by obtaining after cold drying or low temperature dewatering pulverizes or chooses fresh Cordyceps and pulverize the reservation that is conducive to Cordyceps beneficiating ingredient.
Claims (7)
1. a preparation method for aweto micropowder buccal tablet, comprises the following steps:
First; get water content and be not less than 10%(weight) Cordyceps be chilled to 0 ℃ following and pulverize under not higher than the environment of 0 ℃; to pulverize the direct lyophilizing of aweto micropowder of gained, the Cordyceps freeze-dry micropowder water content after lyophilizing is not higher than 3%(weight);
Then; by Cordyceps freeze-dry micropowder rehydration: water ultrasonic atomizatio used rehydration is become in water smoke input freeze-dry micropowder; stir freeze-dry micropowder makes its water content evenly be elevated to 4 ~ 7.9%(weight simultaneously), obtaining water content is 4 ~ 7.9%(weight) rehydration micropowder;
By gained rehydration micropowder tabletting, obtain the pure powder buccal tablet of Cordyceps again.
2. the preparation method of a kind of aweto micropowder buccal tablet according to claim 1, is characterized in that: the Cordyceps before described pulverizing is fresh Cordyceps.
3. the preparation method of a kind of aweto micropowder buccal tablet according to claim 1, is characterized in that: the Cordyceps before described pulverizing is the fresh Cordyceps after dehydration in the low temperature environment below 25 ℃.
4. the preparation method of a kind of aweto micropowder buccal tablet according to claim 1, is characterized in that: after described pulverizing, the aweto micropowder of gained refers to the micropowder of diameter between 0.02 ~ 50 μ m.
5. the preparation method of a kind of aweto micropowder buccal tablet according to claim 1, is characterized in that: the water content of described rehydration micropowder is 5-7.9%(weight).
6. the preparation method of a kind of aweto micropowder buccal tablet according to claim 5, is characterized in that: the water content of described rehydration micropowder is 7%(weight).
7. the preparation method of a kind of aweto micropowder buccal tablet according to claim 6, is characterized in that: described pulverizing is carried out in protective atmosphere.
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| CN103417582B (en) * | 2013-07-29 | 2015-06-10 | 曹静 | Cordyceps sinensis pure powder tablet and preparation method thereof |
| CN103689551B (en) * | 2013-11-25 | 2016-04-20 | 中国林业科学研究院亚热带林业研究所 | The preparation method of the cyclodextrin powder of a kind of enrichment ferfas activity and local flavor and application |
| CN105311063A (en) * | 2014-08-05 | 2016-02-10 | 张锦全 | Cordyceps sinensis tablet and preparation method thereof |
| CN104642688A (en) * | 2015-02-13 | 2015-05-27 | 佛山市宝资林生物科技有限公司 | Preparation method of cordyceps militaris link tableted candy |
| CN105030706A (en) * | 2015-07-08 | 2015-11-11 | 成都易创思生物科技有限公司 | Method for preparing nutrition buccal tablet from Naqu cordyceps sinensis |
| CN105998099A (en) * | 2016-05-19 | 2016-10-12 | 青海悦真生物科技有限公司 | Cordyceps sinensis buccal tablet and preparation method thereof |
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| CN101317562A (en) * | 2008-07-17 | 2008-12-10 | 吕坤秋 | Biological vacuum freezing and drying method for aweto |
| CN102228245A (en) * | 2011-06-24 | 2011-11-02 | 江苏康迪生物科技有限公司 | Granular preparation prepared from ultramicro pure cordycep sporocarp powder and preparation method thereof |
| CN102631377A (en) * | 2012-04-28 | 2012-08-15 | 三普药业股份有限公司 | Cordyceps sinensis freeze-dried nano powder tablet and preparation method thereof |
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| CN101317562A (en) * | 2008-07-17 | 2008-12-10 | 吕坤秋 | Biological vacuum freezing and drying method for aweto |
| CN102228245A (en) * | 2011-06-24 | 2011-11-02 | 江苏康迪生物科技有限公司 | Granular preparation prepared from ultramicro pure cordycep sporocarp powder and preparation method thereof |
| CN102631377A (en) * | 2012-04-28 | 2012-08-15 | 三普药业股份有限公司 | Cordyceps sinensis freeze-dried nano powder tablet and preparation method thereof |
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