CN105769937A - Method for preparing cordyceps sinensis-containing pure powder tablets under low pressure - Google Patents
Method for preparing cordyceps sinensis-containing pure powder tablets under low pressure Download PDFInfo
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Abstract
The invention discloses a method for preparing cordyceps sinensis-containing pure powder tablets under low pressure, belonging to the fields of medicines and health care products. The method provided by the invention adopts cordyceps sinensis original grass with water content less than 8% to prepare micro powder, and comprises the steps of carrying out dry tableting under a condition of 0.1-25kN, enabling the prepared tablets to absorb a certain amount of solvent in a liquid vapor environment of water, an ethyl alcohol solvent or an ethyl acetate solvent, then freezing the tablets under a condition of the temperature being below a melting point of the absorbed solvent, and finally, carrying out freeze drying on the frozen samples to obtain the cordyceps sinensis-containing pure powder tablets. The appearance shapes and parameters such as hardness of the cordyceps sinensis-containing tablets are improved while the quality of the prepared tablets meets a tablet quality standard, the tableting pressure in the existing cordyceps sinensis-containing tablet processing technology is greatly reduced, pore channel structures in the tablets are greatly improved, and the pore volumes, pore areas and porosities of the interiors of the tablets are improved. The tablets prepared by the technology are good in appearance and high in yield, the hardness, frangibility and disintegration of the tablets are in accordance with tablet quality requirements, and relevant parameters of the cordyceps sinensis-containing pure powder tablets prepared by the method are better than those of cordyceps sinensis-containing tablets prepared by the existing high-pressure dry powder tablet processing technology.
Description
Technical field
The invention belongs to medicine and health product technology field, especially by warp again after low pressure compacting Cordyceps pure powder tablet
Absorbed by controllable solvent and lyophilization and prepare the technology of qualified Cordyceps pure powder tablet.
Background technology
Cordyceps (Cordyceps sinensis) is that Hypocreales section ergot fungus cordyceps sinensis bacterium colonizes in squama
Wing mesh Hepialidae Hepialus armorieanus Oberthur belongs to the Stroma on insect larvae and larva cadaveric complex, is mainly distributed on China Qinghai-Tibet Platean
The west and south, Bhutan, Nepal drink on the plateau of Northeastern India height above sea level 3500-5000 rice.Via the development of modern medicine, card
Real its has anticancer, immunomodulating, antioxidation, defying age and diabetes effect, just records it in China's " Bencao Congxin "
There is the effect of " tonifying the lung, kidney tonifying, relieving cough and resolving phlegm, chronic cough ", and be just registered as Chinese tradition by state-promulgated pharmacopoeia as far back as 1964
Chinese medicine, U.S. FDA is also listed in ordinary meal nutrient product.
The Cordyceps product that China's Vehicles Collected from Market is sold, is divided into former grass and deep processed product two class, in deep processed product
It is divided into again compatibility compound type product and the big class of single component type product (pure powder, pure powder tablet) two.Wherein, the pin of the former grass of Cordyceps
Selling and still occupy the bigger market share, and on the deep processed product market of Cordyceps, single component type product is (pure powder, pure
Powder sheet) occupy leader status.In the preparation technology of conventional Cordyceps pure powder tablet, tabletting technology is the most crucial, and research is also
The most deep.The technical research and development of Cordyceps pure powder tablet is to expand to grind on the basis of accumulating other tablet technology of preparing
Send out, in the preparation process of tablet, be generally required for being used in mixed way or add substantial amounts of adjuvant with other medical material in order to compose
Type, wherein one of major reason is that its mechanical strength of tablet, friability and the disintegrating property prepared due to pure raw material cannot
Reach national requirements, it is impossible to meet tablet routine use and circulation demand.Cordyceps is as the extraordinary rare Chinese medicine of a kind of China
Material, its former grass always as famous and precious tonic by compatriots' life-time service, in recent years, the research of its pure powder tablet agent with preparation extensively closed
Note, many researcheres obtain the tablet of single raw material by changing tablet producing technology parameter.Such as " Cordyceps is micro-
Powder sheet and preparation method thereof " preparation method in (ZL200810303308.8) use water content 8~18% and particle diameter 5
~44 aweto micropowders of μm, by first pre-tabletting or/again the method for direct compression (pressure up to 60kN) prepare list
The tablet of one Cordyceps composition;And for example in " a kind of Cordyceps pure powder tablet and preparation method thereof " (CN 103417582 A) ,-10
DEG C extremely low temperature under, prepare pure Cordyceps by the way controlling lower water content (3~7%%) and particle diameter (1~150 μm)
Sheet;It is similar to, " Cordyceps lyophilizing nano powder sheet and preparation method thereof " (CN 102631377 A), uses in water content < 9%
And particle diameter again 10~800nm lyophilized powder in add water be prepared as homogeneous slurry, then use lyophilizing dehydration mode prepare
Obtain Cordyceps sinensis buccal tablets;Other all uses similar fashion about the preparation patent of Cordyceps buccal tablet, joins by changing tablet technique
Numeral system is for Cordyceps pure powder tablet agent.
The preparation of Cordyceps pure powder tablet at present is all mainly by changing the water content parameter of Cordyceps micropowder, by increasing
The pressure of pressure sheet machine, utilize mechanical pressure by powder pressing forming, during the tableting pressure that uses the highest, the highest permissible
Reaching the pressure of 60kN, different film-making pressure can affect the dissolution of tablet[1].High tabletting is conducive to the molding of tablet, full
Hardness in foot tablet listing and friability requirement, but we also simultaneously view, and too high pressure can cause extruding
Tablet is overly hard, decreases the surface area of the porosity within sheet and tablet, thus causes tablet disintegration times to extend even
Defective, it is impossible to meet country's requirement about tablet[2-4]., we have further appreciated that, too high pressure can cause the tightest meanwhile
Cause tablet configuration and be unfavorable for digesting and assimilating of tablet.And tablet prepared by relatively low pressure can keep tablet internal abundant
Pore passage structure, tablet enter internal after increase digesting and assimilating of the contact area of Digestive system and tablet, beneficially tablet.Reason
In opinion, tablet pore passage structure is the abundantest, and after entrance human body, it is more conducive to digesting and assimilating.Therefore, tablet needs in preparation process
Selecting suitable tableting pressure, purpose is contemplated to meet the physical properties such as tablet pattern, hardness, friability and disintegrate simultaneously
Requiring and be conducive to the purpose digested and assimilated, under the physical index of tablet meets the similarity condition of requirement, prepared by tablet
The pressure used in journey is the lowest more is conducive to digesting and assimilating of tablet.In Cordyceps tablet manufacture, there is presently no
A kind of technology can under low pressure be prepared and meet the method that national standard requires tablet, is all under high pressure to be prepared.
Summary of the invention
The technical problem to be solved in the present invention is: overcoming Cordyceps pure powder tablet preparation process mesolow tabletting cannot make
For the deficiency going out qualified Cordyceps pure powder tablet, it is provided that a kind of method preparing Cordyceps pure powder tablet under lower pressure.
The technical solution adopted for the present invention to solve the technical problems is: prepare the pure powder of Cordyceps under a kind of lower pressure
The method of sheet, comprises the steps: first by aweto micropowder compressing dry granulation under 0.1~25kN, then is existed by prepared tablet
The steam ambient of solvent liquid absorbs a certain amount of solvent, freezing, finally by cold below the fusing point of described solvent the most again
Product lyophilization after freezing i.e. obtains aweto micropowder tablet.
Preferably, described solvent includes one or the combination of following solvent: water, ethanol or ethyl acetate.
Preferably, the adsorbance of described solvent is between 0.1%~85% of described tablet quality.
Preferably, the adsorbance of described solvent is between 10.3%~83.5% of described tablet quality.
Preferably, described lyophilization, its baking temperature is :-196 DEG C~-1 DEG C.Further, described lyophilization
Temperature be-196 DEG C~-25 DEG C.
Preferably, described freezing below the fusing point of described solvent, its cryogenic temperature is-120 DEG C~-5 DEG C.
Preferably, described aweto micropowder particle diameter is 0.01~200 μm.Further, described aweto micropowder
Particle diameter is 1.3~150 μm.
Preferably, described micropowder tablet prepare pressure 0.1~23.8kN.Further, the preparation of described micropowder tablet
Pressure is 0.45~23.8kN.
Preferably, described micropowder tablet prepare pressure 0.1~15.9kN.Further, the preparation of described micropowder tablet
Pressure is 0.45~15.9kN.
Preferably, described micropowder tablet prepare pressure 0.1~4.95kN.Further, the preparation of described micropowder tablet
Pressure is 0.45~4.95kN.
Preferably, described micropowder tablet prepare pressure 0.1~2.25kN.Further, the preparation pressure of described micropowder tablet
Power is 0.45~2.25kN.
Preferably, described micropowder tablet prepare pressure 2.25~4.95kN.
Preferably, described micropowder tablet prepare pressure 4.95~15.9kN.
Preferably, the vapour pressure of described solvent liquid is 4.2~70kPa.Further, the vapour pressure of described solvent liquid
It is 7~20kPa.
The invention has the beneficial effects as follows, the low pressure of the present invention prepares the method for Cordyceps pure powder tablet, is based primarily upon selected
In solvent capillary absorption aggregation between tablet micropore and Cordyceps, water solublity or liposoluble constituent produce after dissolving
Cohere ability, the loosest tablet is binded closely, thus under low film-making pressure, obtain the product meeting performance requirement, with
Time the Cordyceps pure powder tablet that prepared by the method for the present invention there is higher porosity, bigger total hole area and total
Pore volume, thus there is shorter disintegration and preferable dissolution.
Accompanying drawing explanation
Fig. 1 is that Cordyceps buccal tablet 1 percentage amounts that absorbs water changes over figure, and wherein abscissa unit is hour, vertical coordinate
Unit is water absorption rate (%);
Fig. 2 is that Cordyceps buccal tablet 2 percentage amounts that absorbs water changes over figure, and wherein abscissa unit is hour, vertical coordinate
Unit is water absorption rate (%);
Fig. 3 be Cordyceps buccal tablet hardness with film-making pressure history figure,;Below in conjunction with the accompanying drawings with embodiment to this
Bright further illustrate.
Fig. 4 is direct compression sample duct scattergram under 39.75kN.
Fig. 5: for the sample duct scattergram of the embodiment of the present invention 1.
Inventor finds in the research of Cordyceps buccal tablet, by the Cordyceps buccal tablet prepared under different film-making pressure its
Different to the absorption property of water, such as inventor uses direct compression process directly to be distinguished by 25~38 μm aweto micropowders
Using compressing dry granulation to prepare sample 1,2 under 0.9kN and 31.8kN pressure, then studying it at steam partial pressure is 20kPa's
Water absorption situation over time under environment, its water absorption is listed in Fig. 1 and Fig. 2 over time.From Fig. 1 and Fig. 2 we
It can be seen that the adsorbance that Cordyceps buccal tablet is to moisture content, within the certain time being exposed to water vapor, it is to moisture content
Adsorbance can increase over time and increase, and in being exposed to water vapour, after certain time, its adsorbance reaches balance, substantially
Stable in certain ratio.And this absorbability can be due to film-making condition, such as film-making pressure, difference and cause it right
The absorption property of moisture content can be different.
Simultaneously as it is shown on figure 3, in the hardness research of Cordyceps buccal tablet, it has been found that the hardness of Cordyceps buccal tablet with
The increase of film-making pressure and increase, such as inventor uses direct compression process directly to be distinguished by 25~38 μm aweto micropowders
Using compressing dry granulation film-making at various pressures, then study its tablet hardness situation of change with film-making pressure, its data arrange
In Fig. 3.Data from figure, we can see that big film-making pressure is conducive to increasing tablet hardness, and low film-making pressure are not
It is beneficial to the increase of tablet hardness, so presently commercially available Cordyceps product is all the product prepared under high pressure.But, high
Film-making pressure is unfavorable for digesting and assimilating of tablet.Therefore, in the case of keeping tablet hardness isoparametric, tablet film-making pressure is more
Low the best.
Fig. 4,5 respectively list employing the direct compressing dry granulation of 39.75kN and use the inventive method under 0.45kN pressure
Prepare the contrast pore distribution figure of tablet, by Data Comparison in figure it can be seen that its hole of tablet of preparing of the inventive method
Road is distributed the tablet at relative 39.75kN direct compressing dry granulation preparation, and it has two obvious ducts at 9000nm, 8000nm
Distribution of peaks, illustrates that the tablet that the inventive method prepares has the duct of more horn of plenty, and therefore, we also can draw the present invention
Method enriches the conclusion of the internal gutter structure of tablet greatly.
Detailed description of the invention
Presently in connection with example, the present invention is further detailed explanation.These embodiments illustrate this most by way of example
The substance of invention, therefore it only shows the composition relevant with the present invention.
Embodiment 1:
The concrete preparation method of this example is as follows:
(1): the former grass meal of Cordyceps that water content is less than 8% is broken to the powder that particle diameter is 48~75 μm, at room temperature
By compressing dry granulation, controlling to be pressed into by Cordyceps powder under conditions of tableting pressure is 0.45kN the sheet of a diameter of 10mm
Agent;
(2) the Cordyceps tablet of above-mentioned preparation is placed in the water vapour environment that vapour pressure is about 20kPa water suction 12 hours,
Making Cordyceps tablet is the 27.2% of deadweight to the adsorbance of water;
(3) immediately the Cordyceps tablet after water suction is put into freezing 10 hours of the environment of-5 DEG C, until the liquid in sample
State water all forms the ice of solid-state;
(4) tablet after freezing is placed in temperature for lyophilization at a temperature of-25 DEG C to constant weight.
Sample analysis:
1. sample sample preparation repeatability is linear investigates
Repeat above-mentioned Sample Preparation Procedure, and prepare 24 samples, understand this batch sample sample preparation success rate by experiment
More than more than 95%.And utilize and be accurate to its weight of electronic scale weighing of 0.1mg, and note down the weight of each sample, its experiment
Result is as shown in table 1, and the standard deviation being calculated gained sample by standard deviation calculation formula formula (1) is 0.0027, sample
Preparation repeatability is good.
Represent sample X1, the X2 used ..., the average (1) of Xn
Table 1: Cordyceps sample quality table prepared by low pressure tabletting
Sample number into spectrum | Example weight (g) |
1 | 0.2511 |
2 | 0.2485 |
3 | 0.2472 |
4 | 0.2521 |
5 | 0.2500 |
6 | 0.2510 |
7 | 0.2449 |
8 | 0.2495 |
9 | 0.2489 |
10 | 0.2551 |
11 | 0.2570 |
12 | 0.2551 |
13 | 0.2480 |
14 | 0.2501 |
15 | 0.2521 |
16 | 0.2510 |
17 | 0.2530 |
18 | 0.2502 |
19 | 0.2498 |
20 | 0.2531 |
21 | 0.2501 |
22 | 0.2479 |
23 | 0.2498 |
24 | 0.2469 |
2. tablet hardness test
Initially with identical aweto micropowder direct compression process, tableting pressure respectively at 0.45kN and 39.75kN,
Prepare 24 samples respectively, use 24 samples that the inventive method is prepared under 0.45kN tableting pressure as contrast simultaneously
Test.Then use YD-1 type tablet hardness instrument test above-mentioned preparation be used for contrast Cordyceps buccal tablet and the inventive method system
Standby go out sample hardness, and calculate its meansigma methods for contrasting, experimental result is listed in table 2. as can be seen from the table,
Pressure be 0.45kN low pressure under the tablet hardness that goes out of direct compression only have 0.09Kg, it is impossible to meet the foot needed for tablet commercialization
Enough hardness, therefore commercially produced product is all to use high-pressure process to prepare.From table, we are it can also be seen that be 39.75kN at pressure
High pressure under direct compression tablet hardness reach 2.21Kg, significantly larger than under low pressure obtain tablet hardness.And the inventive method
The tablet prepared under the extremely low pressure of 0.45kN, its hardness is up to 2.53Kg, and its effect is even above high pressure 39.75kN pressure
The tablet prepared under power.Therefore, the inventive method has the beneficial effect significantly improving tablet hardness.
Table 2: different flaking method tablet hardness comparing results
3. tablet friability test
Initially with identical aweto micropowder direct compression process, tableting pressure respectively at 0.45kN and 39.75kN,
Prepare 24 samples respectively, use 24 samples that this inventive method is prepared as contrast test simultaneously.Then CS-2 is used
Type tablet friability tester, uses 25 revs/min, the above-mentioned friability preparing sample of condition test of turntable rotation 100 circle, and
Calculating its meansigma methods for contrasting, experimental result is listed in table 3.From table, we are it can also be seen that be 39.75kN's at pressure
Under high pressure, direct compression tablet friability reaches 1.2%, tablet 15.6% friability obtained under low pressure.And this
The tablet that bright method is prepared under the extremely low pressure of 0.45kN, its friability only has 0.1%, and its effect is even above under high pressure
The tablet prepared, low friability explanation tablet not cracky when in market circulation.Therefore, the inventive method has substantially
Improve the beneficial effect of tablet friability.
Table 3: different flaking method tablet friability comparing results
4. disintegration of tablet test
Initially with identical aweto micropowder direct compression process, tableting pressure respectively at 0.45kN and 39.75kN,
Prepare 24 samples respectively, use 24 samples that this inventive method is prepared as contrast test simultaneously.Then BJ-1 is used
Matrix agent disintegration time tester, the condition test that uses cage lifting frequency to be 30 beats/min and water temperature 37 DEG C is above-mentioned prepares sample
Disintegration, and calculate its meansigma methods for contrasting, experimental result is listed in table 4.From table, we are it can also be seen that pressing
Power be 39.75kN high pressure under time-consuming 15 minutes of direct compression disintegration of tablet, higher than the tablet disintegrate of 1 minute obtained under low pressure
Time limit.And the tablet that the inventive method is prepared under the extremely low pressure of 0.45kN, time-consuming 10 minutes of its disintegrate, each disintegration of tablet
Test all meets the national prescription about the disintegration of tablet time limit within 30 minutes.Therefore, the inventive method has reduction
The beneficial effect in Cordyceps disintegration of tablet time limit.
Table 4: different flaking method disintegration of tablet time limit comparing results
5. tablet pore distribution test
Initially with identical aweto micropowder direct compression process, tableting pressure respectively at 0.45kN and 39.75kN,
Prepare sample respectively, use sample prepared by this inventive method as contrast test simultaneously.Then AutoPore IV is used
The pore distribution of 9500 mercury injection apparatus test samples.From the test result of sample it can be seen that use the inventive method to synthesize
The total hole area of Cordyceps is prepare tablet under 39.75kN 8.5 times, and total pore volume is to prepare the 1.7 of slice under 39.75kN
Times, porosity is then prepare tablet under 39.75kN 1.3 times, it is seen that the technology described in the inventive method can be greatly improved
With the contact area of Digestive system during tablet digestion, it is substantially improved the pore passage structure of tablet.
Table 5: tablet pore distribution test result
Embodiment 2:
The concrete preparation method of this example is as follows:
(1): the former grass meal of Cordyceps that water content is less than 8% is broken to the powder that particle diameter is 58~150 μm, at room temperature
By compressing dry granulation, controlling to be pressed into by Cordyceps powder under conditions of tableting pressure is 2.25kN the sheet of a diameter of 10mm
Agent.
(2) the Cordyceps tablet of above-mentioned preparation is placed in the water vapour environment that vapour pressure is about 15kPa water suction 12 hours,
Making Cordyceps tablet is the 41.7% of deadweight to the adsorbance of water.
(3) immediately the Cordyceps tablet after water suction is put into freezing 12 hours of the environment of-5 DEG C, until the liquid in sample
State water all forms the ice of solid-state.
(4) tablet after freezing is set at a temperature of-25 DEG C lyophilization to constant weight as temperature.
Sample analysis:
1. tablet hardness test
Initially with identical aweto micropowder direct compression process, tableting pressure respectively at 2.25kN and 39.75kN,
Prepare 24 samples respectively, use 24 samples that this inventive method is prepared as contrast test simultaneously.Then YD-1 is used
Type tablet hardness instrument test above-mentioned preparation for contrasting Cordyceps buccal tablet and the inventive method prepares the hardness of sample, and
Calculating its meansigma methods for contrasting, experimental result is listed in table 6.As can be seen from the table, it is the low of 2.25kN at pressure
The tablet hardness that pressure direct compression goes out only has 0.65Kg, it is impossible to meet the enough hardness needed for tablet commercialization.From table I
It can also be seen that under the high pressure that pressure is 39.75kN direct compression tablet hardness reach 2.02Kg, higher than under low pressure obtain
Tablet hardness.And the tablet that the inventive method is prepared under the low-pressure of 2.25kN, its hardness is up to 5.41Kg, its hardness
It it is 2.7 times of the tablet prepared under high pressure.Therefore, the inventive method has the beneficial effect significantly improving tablet hardness.
The different flaking method tablet hardness comparing result of table 6
2. tablet friability test
Initially with identical aweto micropowder direct compression process, tableting pressure respectively at 2.25kN and 39.75kN,
Prepare 24 samples respectively, use 24 samples that this inventive method is prepared under 2.25kN tabletting conditions as contrast simultaneously
Test.Then use CS-2 type tablet friability tester, use 25 revs/min, the above-mentioned system of condition test of turntable rotation 100 circle
The friability of standby sample, and calculate its meansigma methods for contrasting, experimental result is listed in table 7.From table we it can also be seen that
Under the high pressure that pressure is 39.75kN, direct compression tablet friability reaches 1.5%, less than the tablet 3.2% obtained under low pressure
Friability.And the tablet that the inventive method is prepared under the low-pressure of 2.25kN, its friability is less than 0.1%, and effect is higher than
The tablet prepared under high pressure, low friability explanation tablet not cracky when in market circulation.Therefore, the inventive method tool
Have clear improvement the beneficial effect of tablet friability.
Table 7: different flaking method tablet friability comparing results
3. disintegration of tablet test
Initially with identical aweto micropowder direct compression process, tableting pressure respectively at 2.25kN and 39.75kN,
Prepare 24 samples respectively, use this inventive method to prepare 24 samples under 2.25kN tabletting conditions simultaneously and survey as contrast
Examination.Then BJ-1 matrix agent disintegration time tester is used, the condition survey using cage lifting frequency to be 30 beats/min and water temperature 37 DEG C
Trying the above-mentioned disintegration preparing sample, and calculate its meansigma methods for contrasting, experimental result is listed in table 8.From table we
It can also be seen that under the high pressure that pressure is 39.75kN time-consuming 13 minutes of direct compression disintegration of tablet, higher than under low pressure obtain
Tablet disintegration of 4 minutes.And the tablet that the inventive method is prepared under the low-pressure of 2.25kN, time-consuming 12 points of its disintegrate
Clock, meets the national prescription about the disintegration of tablet time limit within 30 minutes.Therefore, the inventive method has reduction winter worm
The beneficial effect of summer blade agent disintegration.
Table 8: different flaking method disintegration of tablet time limit comparing results
Embodiment 3:
The concrete preparation method of this example is as follows:
(1): the former grass meal of Cordyceps that water content is less than 8% is broken to the powder that particle diameter is 25~38 μm, at room temperature
By compressing dry granulation, controlling to be pressed into by Cordyceps powder under conditions of tableting pressure is 4.95kN the sheet of a diameter of 10mm
Agent.
(2) the Cordyceps tablet of above-mentioned preparation is placed in the water vapour environment that vapour pressure is about 10kPa water suction 12 hours,
Making Cordyceps tablet is the 22.7% of deadweight to the adsorbance of water.
(3) immediately the Cordyceps tablet after water suction is put into freezing 24 hours of the environment of-5 DEG C, until the liquid in sample
State water all forms the ice of solid-state.
(4) tablet after freezing is set at a temperature of-25 DEG C lyophilization to constant weight as temperature.
Sample analysis:
1. tablet hardness test
Initially with identical aweto micropowder direct compression process, tableting pressure respectively at 4.95kN and 39.75kN,
Preparing 24 samples respectively, 24 samples simultaneously using this inventive method to prepare under the conditions of 4.94kN are surveyed as contrast
Examination.Then use YD-1 type tablet hardness instrument test above-mentioned preparation be used for contrast Cordyceps buccal tablet and prepared by the inventive method
Going out the hardness of sample, and calculate its meansigma methods for contrasting, experimental result is listed in table 9.As can be seen from the table, in pressure
Power be 4.95kN low pressure under the tablet hardness that goes out of direct compression only have 1.59Kg, it is impossible to meet needed for tablet commercialization is enough
Hardness.From table we it can also be seen that under the high pressure that pressure is 39.75kN direct compression tablet hardness reach 2.33Kg,
It is significantly larger than under low pressure the tablet hardness obtained.And the tablet that the inventive method is prepared under the extremely low pressure of 4.95kN, its
Hardness is up to 6.37Kg, and its effect is 2.7 times of the hardness preparing tablet under high pressure.Therefore, the inventive method has substantially
Improve the beneficial effect of tablet hardness.
Table 9: different flaking method tablet hardness comparing results
2. tablet friability test
Initially with identical aweto micropowder direct compression process, tableting pressure respectively at 4.95kN and 39.75kN,
Preparing 24 samples respectively, 24 samples simultaneously using this inventive method to prepare under the conditions of 4.95kN are surveyed as contrast
Examination.Then use CS-2 type tablet friability tester, use 25 revs/min, the above-mentioned preparation of condition test of turntable rotation 100 circle
The friability of sample, and calculate its meansigma methods for contrasting, experimental result is listed in table 10.From table we it can also be seen that
Under the high pressure that pressure is 39.75kN, direct compression tablet friability reaches 1.1%, less than the tablet 2.5% obtained under low pressure
Friability.And the tablet that the inventive method is prepared under the extremely low pressure of 4.95kN, its friability is only less than 0.1%, its
The tablet prepared under effect even above high pressure, low friability explanation tablet not cracky when in market circulation.Therefore,
The inventive method has the beneficial effect being obviously improved tablet friability.
Table 10: different flaking method tablet friability comparing results
3. disintegration of tablet test
Initially with identical aweto micropowder direct compression process, tableting pressure respectively at 4.95kN and 39.75kN,
Prepare 24 samples respectively, use this inventive method to prepare 24 samples under 4.95kN tabletting conditions simultaneously and survey as contrast
Examination.Then BJ-1 matrix agent disintegration time tester is used, the condition survey using cage lifting frequency to be 30 beats/min and water temperature 37 DEG C
Trying the above-mentioned disintegration preparing sample, and calculate its meansigma methods for contrasting, experimental result is listed in table 11.From table we
It can also be seen that under the high pressure that pressure is 39.75kN time-consuming 17 minutes of direct compression disintegration of tablet, higher than under low pressure obtain
Tablet disintegration of 7 minutes.And the tablet that the inventive method is prepared under the low-pressure of 4.95kN, time-consuming 13 points of its disintegrate
Clock, meets the national prescription about the disintegration of tablet time limit within 30 minutes.Therefore, the inventive method has reduction winter worm
The beneficial effect of summer blade agent disintegration.
Table 11: different flaking method disintegration of tablet time limit comparing results
Embodiment 4:
The concrete preparation method of this example is as follows:
(1): the former grass meal of Cordyceps that water content is less than 8% is broken to the powder that particle diameter is 1.3~6.5 μm, in room temperature
Under by compressing dry granulation, under conditions of tableting pressure is 23.8kN, Cordyceps powder is pressed into a diameter of 10mm's controlling
Tablet;
(2) the Cordyceps tablet of above-mentioned preparation is placed in the water vapour environment that vapour pressure is about 7kPa water suction 24 hours,
Making Cordyceps tablet is the 83.5% of deadweight to the adsorbance of water;
(3) immediately the Cordyceps tablet after water suction is put into freezing 3 hours of the environment of-5 DEG C, until the liquid in sample
Water all forms the ice of solid-state;
(4) tablet after freezing is set at a temperature of-25 DEG C lyophilization to constant weight as temperature.
Sample analysis:
1. tablet hardness test
Initially with identical aweto micropowder direct compression process, tableting pressure respectively at 23.8kN and 39.75kN,
Prepare 24 samples respectively, use the inventive method to prepare 24 samples under 23.8kN pressure as contrast test simultaneously.
Then use YD-1 type tablet hardness instrument to test the hardness sample of above-mentioned preparation, and calculate its meansigma methods for contrasting,
Experimental result is listed in table 12.As can be seen from the table, the tablet that direct compression goes out under the low pressure that pressure is 23.8kN is hard
Degree is 2.31Kg, and under the high pressure that pressure is 39.75kN, direct compression tablet hardness reaches 2.52Kg, and the inventive method exists
The tablet prepared under the pressure of 23.8kN, its hardness is up to 8.03Kg, and hardness dramatically increases.Therefore, the inventive method tool
The beneficial effect of the tablet hardness that is significantly improved.
Table 12: different flaking method tablet hardness comparing results
2. tablet friability test
Initially with identical aweto micropowder direct compression process, tableting pressure respectively at 23.8kN and 39.75kN,
Preparing 24 samples respectively, 24 samples simultaneously using this inventive method to prepare under conditions of 23.8kN are surveyed as contrast
Examination.Then use CS-2 type tablet friability tester, use 25 revs/min, the above-mentioned preparation of condition test of turntable rotation 100 circle
The friability of sample, and calculate its meansigma methods for contrasting, experimental result is listed in table 13.From table we it can also be seen that
Under the pressure that pressure is 39.75kN, direct compression tablet friability reaches 1.0%, becomes blind its tablet friability at 23.8kN pressure
It is 1.7%, and the tablet that the inventive method is prepared under the pressure of 23.8kN, its friability is less than 0.1%, and its effect is better than
The tablet that reduced pressure is prepared, low friability explanation tablet not cracky when in market circulation.Therefore, the inventive method
There is the beneficial effect being obviously improved tablet friability.
Table 13: different flaking method tablet friability comparing results
3. disintegration of tablet test
Initially with identical aweto micropowder direct compression process, tableting pressure respectively at 23.8kN and 39.75kN,
Prepare 24 samples respectively, use this inventive method to prepare 24 samples under 23.8kN tabletting conditions simultaneously and survey as contrast
Examination.Then BJ-1 matrix agent disintegration time tester is used, the condition survey using cage lifting frequency to be 30 beats/min and water temperature 37 DEG C
Trying the above-mentioned disintegration preparing sample, and calculate its meansigma methods for contrasting, experimental result is listed in table 14.From table we
It can also be seen that under the high pressure that pressure is 39.75kN time-consuming 19 minutes of direct compression disintegration of tablet, higher than 23.8kN film-making pressure
The tablet disintegration of 12 minutes obtained under power.The tablet that the inventive method is prepared under the low-pressure of 23.8kN, it collapses
Solve time-consuming 14 minutes, meet the national prescription about the disintegration of tablet time limit within 30 minutes.
Table 14: different flaking method disintegration of tablet time limit comparing results
Embodiment 5:
The concrete preparation method of this example is as follows:
(1): the former grass meal of Cordyceps that water content is less than 8% is broken to the powder that particle diameter is 13~25 μm, at room temperature
By compressing dry granulation, controlling to be pressed into by Cordyceps powder under conditions of tableting pressure is 15.9kN the sheet of a diameter of 10mm
Agent;
(2) the Cordyceps tablet of above-mentioned preparation is placed in the alcohol vapor environment that vapour pressure is about 13.3kPa absorption
12 hours so that Cordyceps tablet is the 40.8% of deadweight to the adsorbance of ethanol;
(3) the Cordyceps tablet after ethanol will be absorbed immediately and put into freezing 12 hours of the environment of-120 DEG C, until sample
In liquid ethanol all solidify;
(4) tablet after freezing is set at a temperature of-196 DEG C lyophilization to constant weight as temperature.
Sample analysis:
1. tablet hardness test
Initially with identical aweto micropowder direct compression process, tableting pressure respectively at 15.9kN and 39.75kN,
Preparing 24 samples respectively, 24 samples simultaneously using this inventive method to prepare under the pressure of 15.9kN are surveyed as contrast
Examination.Then use YD-1 type tablet hardness instrument test above-mentioned preparation be used for contrast Cordyceps buccal tablet and prepared by the inventive method
Going out the hardness of sample, and calculate its meansigma methods for contrasting, experimental result is listed in table 15.As can be seen from the table, exist
Pressure be 15.9kN pressure under the tablet hardness that goes out of direct compression only have 2.12Kg.From table, we are it can also be seen that pressing
Power be 39.75kN high pressure under direct compression tablet hardness reach 2.19Kg, higher than under low pressure obtain tablet hardness.And this
The tablet that bright method is prepared under the pressure of 15.9kN, its hardness is up to 8.67Kg, and its hardness is to prepare tablet under high pressure
Nearly 4 times of hardness.Therefore, the inventive method has the beneficial effect significantly improving tablet hardness.
Table 15: different flaking method tablet hardness comparing results
2. tablet friability test
Initially with identical aweto micropowder direct compression process, tableting pressure respectively at 15.9kN and 39.75kN,
Prepare 24 samples respectively, use 24 samples that this inventive method is prepared as contrast test simultaneously.Then CS-2 is used
Type tablet friability tester, uses 25 revs/min, the above-mentioned friability preparing sample of condition test of turntable rotation 100 circle, and
Calculating its meansigma methods for contrasting, experimental result is listed in table 16.From table, we are it can also be seen that be 39.75kN at pressure
Pressure under direct compression tablet friability reach 1.1%, less than 2.1% friability obtaining tablet under 15.9kN pressure.And
The tablet that the inventive method is prepared under the pressure of 15.9kN, its friability is less than 0.1%, and its effect is even above under high pressure
The tablet prepared, low friability explanation tablet not cracky when in market circulation.Therefore, the inventive method has substantially
Improve the beneficial effect of tablet friability.
Table 16: different flaking method tablet friability comparing results
3. disintegration of tablet test
Initially with identical aweto micropowder direct compression process, tableting pressure respectively at 15.9kN and 39.75kN,
Prepare 24 samples respectively, use this inventive method to prepare 24 samples under 15.9kN tabletting conditions simultaneously and survey as contrast
Examination.Then BJ-1 matrix agent disintegration time tester is used, the condition survey using cage lifting frequency to be 30 beats/min and water temperature 37 DEG C
Trying the above-mentioned disintegration preparing sample, and calculate its meansigma methods for contrasting, experimental result is listed in table 17.From table we
It can also be seen that under the high pressure that pressure is 39.75kN time-consuming 14 minutes of direct compression disintegration of tablet, higher than under 15.9kN pressure
The tablet disintegration of 9 minutes obtained.And the tablet that the inventive method is prepared under the low-pressure of 15.9kN, its disintegrate consumes
Time 10 minutes, meet country about disintegration of tablet time limit prescription within 30 minutes.Therefore, the inventive method has fall
The beneficial effect in low Cordyceps disintegration of tablet time limit.
Table 17: different flaking method disintegration of tablet time limit comparing results
Embodiment 6:
The concrete preparation method of this example is as follows:
(1): the former grass meal of Cordyceps that water content is less than 8% is broken to the powder that particle diameter is 6.5~13 μm, at room temperature
By compressing dry granulation, controlling to be pressed into by Cordyceps powder under conditions of tableting pressure is 23.8kN the sheet of a diameter of 10mm
Agent;
(2) the Cordyceps tablet of above-mentioned preparation is placed in the butanol vapor environment that vapour pressure is about 9.7kPa suction
Receive 12 hours so that Cordyceps tablet is the 10.3% of deadweight to the adsorbance of ethyl acetate;
(3) the Cordyceps tablet after ethyl acetate will be absorbed immediately and put into freezing 12 hours of the environment of-100 DEG C, until
Liquid ethanol in sample all solidifies;
(4) tablet after freezing is set at a temperature of-196 DEG C lyophilization to constant weight as temperature.
Sample analysis:
1. tablet hardness test
Initially with identical aweto micropowder direct compression process, tableting pressure respectively at 23.8kN and 39.75kN,
Preparing 24 samples respectively, 24 samples simultaneously using this inventive method to prepare under 23.8kN pressure are surveyed as contrast
Examination.Then use YD-1 type tablet hardness instrument test above-mentioned preparation be used for contrast Cordyceps buccal tablet and prepared by the inventive method
Going out the hardness of sample, and calculate its meansigma methods for contrasting, experimental result is listed in table 18.As can be seen from the table, exist
Pressure be 23.8kN low pressure under the tablet hardness that goes out of direct compression only have 1.68Kg, we are it can also be seen that at pressure be
Under the high pressure of 39.75kN, direct compression tablet hardness reaches 1.98Kg, the tablet hardness obtained under slightly above 23.8kN pressure.And
The tablet that the inventive method is prepared under the pressure of 23.8kN, its hardness is up to 3.60Kg, and its effect exceeds to be prepared under high pressure
Go out the hardness of tablet.Therefore, the inventive method has the beneficial effect significantly improving tablet hardness.
Table 18: different flaking method tablet hardness comparing results
2. tablet friability test
Initially with identical aweto micropowder direct compression process, tableting pressure respectively at 23.8kN and 39.75kN,
Preparing 24 samples respectively, 24 samples simultaneously using this inventive method to prepare under the conditions of 23.8kN are surveyed as contrast
Examination.Then use CS-2 type tablet friability tester, use 25 revs/min, the above-mentioned preparation of condition test of turntable rotation 100 circle
The friability of sample, and calculate its meansigma methods for contrasting, experimental result is listed in table 19.From table we it can also be seen that
Under the high pressure that pressure is 39.75kN, direct compression tablet friability reaches 1.5%, less than obtaining tablet under 23.8kN pressure
The friability of 1.8%.And the tablet that the inventive method is prepared under the pressure of 23.8kN, its friability only has 0.6%, its effect
The tablet prepared under fruit even above high pressure, low friability explanation tablet not cracky when in market circulation.Therefore, originally
Inventive method has the beneficial effect being obviously improved tablet friability.
Table 19: different flaking method tablet friability comparing results
3. disintegration of tablet test
Initially with identical aweto micropowder direct compression process, tableting pressure respectively at 23.8kN and 39.75kN,
Prepare 24 samples respectively, use this inventive method to prepare 24 samples under 23.8kN tabletting conditions simultaneously and survey as contrast
Examination.Then BJ-1 matrix agent disintegration time tester is used, the condition survey using cage lifting frequency to be 30 beats/min and water temperature 37 DEG C
Trying the above-mentioned disintegration preparing sample, and calculate its meansigma methods for contrasting, experimental result is listed in table 20.From table we
It can also be seen that under the high pressure that pressure is 39.75kN time-consuming 13 minutes of direct compression disintegration of tablet, higher than under low pressure obtain
Tablet disintegration of 11 minutes.And the tablet that the inventive method is prepared under the low-pressure of 23.8kN, its disintegrate time-consuming 10
Minute, meet the national prescription about the disintegration of tablet time limit within 30 minutes.Therefore, the inventive method has the reduction winter
The beneficial effect of worm summer blade agent disintegration.
Table 20: different flaking method disintegration of tablet time limit comparing results
With above-mentioned foundation embodiments of the invention for enlightenment, by above-mentioned description, relevant staff completely may be used
With in the range of without departing from this invention technological thought, carry out various change and amendment.The technical model of this invention
Enclosing the content being not limited in description, all documents that the present invention mentions are incorporated as reference the most in this application, as
It is individually recited as with reference to like that with each document.
List of references:
[1] Chen Zhi, Lee passes sound, " Anhui medicine ", and 2014 (7);1220-1222.
[2] Hao Limin, Wang Yu, Li Zheng, Jia Shiru, Xing Xinhui, " Food Science ", 2006,27 (12);381-384.
The research that tablet quality is affected by the technological parameter with tabletting of [3] pelletizing, Gao Zhijiang, " University Of Tianjin ", 2006.
[4] about the technological parameter pelletized with tabletting on researching and analysing that tablet quality affects, Li Ran, Li Sijie, " China
Health nutrient publication appearing once every ten days ", 2014
Attached performance can be different.
Claims (10)
1. the method that a low pressure prepares aweto micropowder tablet, it is characterised in that: first by aweto micropowder at 0.1 ~ 25kN
Lower compressing dry granulation, more prepared tablet is adsorbed in the steam ambient of solvent liquid a certain amount of solvent, the most again described
Below the fusing point of solvent, freezing, finally i.e. obtains aweto micropowder tablet by the product lyophilization after freezing.
Low pressure the most according to claim 1 prepares the method for Cordyceps aweto micropowder tablet, it is characterised in that: described
Solvent include one or the combination of following solvent: water, ethanol or ethyl acetate.
Low pressure the most according to claim 1 prepares the method for Cordyceps aweto micropowder tablet, it is characterised in that: described
The adsorbance of solvent is between the 0.1% ~ 85% of described tablet quality.
Low pressure the most according to claim 3 prepares the method for Cordyceps aweto micropowder tablet, it is characterised in that: described
The adsorbance of solvent is between the 10.3% ~ 83.5% of described tablet quality.
Low pressure the most according to claim 1 prepares the method for Cordyceps aweto micropowder tablet, it is characterised in that: described
Lyophilization, its baking temperature is :-196 ° of C ~-1 ° C.
Low pressure the most according to claim 1 prepares the method for Cordyceps aweto micropowder tablet, it is characterised in that: described
Aweto micropowder particle diameter be 0.01 ~ 200 μm.
Low pressure the most according to claim 1 prepares the method for aweto micropowder tablet, it is characterised in that: described micropowder tablet
Prepare pressure at 0.1 ~ 23.8kN.
Low pressure the most according to claim 7 prepares the method for Cordyceps aweto micropowder tablet, it is characterised in that: described
Micropowder tablet prepare pressure at 0.1 ~ 15.9kN.
Low pressure the most according to claim 8 prepares the method for Cordyceps aweto micropowder tablet, it is characterised in that: described
Micropowder tablet prepare pressure at 0.1 ~ 4.95kN.
10. the method preparing Cordyceps aweto micropowder tablet according to the low pressure described in any one of claim 1-9, its feature
It is: the vapour pressure of described solvent liquid is 4.2 ~ 70kPa.
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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 |
CN103271953A (en) * | 2013-06-26 | 2013-09-04 | 通化臻尊生物科技有限公司 | Preparation method of high-hardness cordyceps sinensis pure powder tablet |
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US20030133946A1 (en) * | 2001-09-21 | 2003-07-17 | Keith Alec D. | Oral supplement composition containing a plurality of mushroom strains |
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 |
CN103271953A (en) * | 2013-06-26 | 2013-09-04 | 通化臻尊生物科技有限公司 | Preparation method of high-hardness cordyceps sinensis pure powder tablet |
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