CN107898916A - Method for processing bulbus fritilariae and bulbus fritilariae preparation - Google Patents
Method for processing bulbus fritilariae and bulbus fritilariae preparation Download PDFInfo
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- CN107898916A CN107898916A CN201711395394.5A CN201711395394A CN107898916A CN 107898916 A CN107898916 A CN 107898916A CN 201711395394 A CN201711395394 A CN 201711395394A CN 107898916 A CN107898916 A CN 107898916A
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- A61K36/18—Magnoliophyta (angiosperms)
- A61K36/88—Liliopsida (monocotyledons)
- A61K36/896—Liliaceae (Lily family), e.g. daylily, plantain lily, Hyacinth or narcissus
- A61K36/8966—Fritillaria, e.g. checker lily or mission bells
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- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2236/00—Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
- A61K2236/10—Preparation or pretreatment of starting material
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Abstract
The invention provides a method for processing bulbus fritilariae and a bulbus fritilariae preparation, wherein the method for processing the bulbus fritilariae comprises the following steps: (1) slicing or coarsely crushing the bulbus fritilariae, adding an ethanol extracting solution of the rosa davurica pall, and soaking for 1-2 hours at room temperature, wherein the adding amount of the ethanol extracting solution of the rosa davurica pall at least exceeds the bulbus fritilariae; (2) drying the bulbus fritilariae at 70-100 ℃ until the water content is lower than 8%; (3) and micronizing the dried bulbus fritilariae at the temperature of between 35 ℃ below zero and 25 ℃ below zero until more than 95 percent of bulbus fritilariae ultrafine powder has the particle size of 400 to 600 meshes. The bulbus fritilariae processed by the method not only can inhibit browning, increase the elution amount of alkaloid and saponin and improve the drug effect, but also has the advantages of energy conservation, low cost and high cost performance.
Description
Technical field
The present invention relates to Chinese medicine manufacture field, in particular to a kind of method and tendril-leaved fritillary bulb preparation for processing tendril-leaved fritillary bulb.
Background technology
Tendril-leaved fritillary bulb is liliaceous plant bulbus fritillariae cirrhosae F.cirrhosa D.Don, Fritillaria unibracteata F.unibracteata Hsiao
The drying squama of et K.C.Hsia, Gansu fritillaria F.przewalskii Maxim. and Bulbus Fritillariae cirrhosae F.delavayi Franch
Stem, belongs to the traditional rare traditional Chinese medicine in China.Starch is the main component in tendril-leaved fritillary bulb, and account for its gross mass 40~60% are left
The right side, remaining principal component includes cellulose, protein and aliphatic acid etc., and the medicinal ingredient of tendril-leaved fritillary bulb then mainly includes alkaloid, soap
Glycosides and some terpenes and steroidal substances.
Chinese medicine ancient books and records《The southern regions of the Yunnan Province book on Chinese herbal medicine》One secretary carries, and bulbus fritillariae cirrhosae has the function that clearing heat and moistening lung and preventing phlegm from forming and stopping coughing.Modern medicine
Pharmacological research also confirms that, tendril-leaved fritillary bulb can diastole bronchus smooth muscle, have the function that to relieving asthma, antibechic and eliminating the phlegm；Tendril-leaved fritillary bulb can also drop
Blood pressure, reducing heart rate and suppression platelet aggregation, relaxation intestinal contraction, slow down gastrointestinal peristalsis and antiulcer；In addition, tendril-leaved fritillary bulb
Also Central nervous system, respiratory tract infection and tumour have certain therapeutic effect.
In view of how the above-mentioned valuable pharmacological effect of tendril-leaved fritillary bulb, avoid active pharmaceutical ingredient in tendril-leaved fritillary bulb from failing in process
And active pharmaceutical ingredient dissolution is promoted to be of great significance.Traditional tendril-leaved fritillary bulb processing method is will to be crushed after tendril-leaved fritillary bulb high temperature drying
High temperature drying after cutting into slices into coarse granule or by tendril-leaved fritillary bulb, promotes active pharmaceutical ingredient alkaloid using preceding by way of adding water to cook
With the release of saponin(e etc..There are larger defect for this traditional processing mode.First, coarse crushing or section cannot effectively destroy river
The cell membrane of shellfish, is unfavorable for the dissolution of active ingredient.Secondly as the content of starch is high, in the drying process, tendril-leaved fritillary bulb is easily sent out
Raw brown stain, influences the content of active ingredient.Therefore, it is necessary to traditional tendril-leaved fritillary bulb processing method is improved.
Superfine communication technique is nearly new and high technology developed rapidly for 20 years, has uniqueness in Chinese medicine manufacture field
Advantage, can improve the cell-wall breaking ratio of Chinese medicine, specific surface area increase, particle diameter reaches micron order, effectively improve Chinese medicine
The utilization rate of material, strengthens curative effect of medication.And the broken technology of low-temperature submicron powder be grow up on the basis of superfine communication technique it is new
Type crushing technology, the technology operate at low temperature, can effectively reduce the inactivation of heat-sensitive substance in Chinese medicine, reduce volatile
The loss of component, while also it is avoided that the defects of polysaccharose substance is easily adhered in crushing process.
But either conventional superfine communication technique, or the broken technology of low-temperature submicron powder, for different Chinese medicines, ultra micro
The optimum process condition difference of crushing is big, and specific processing effect is also totally different, and some Chinese medicines are even difficult to what is overcome due to existing
Technical problem and be not suitable for being processed using above-mentioned technology.Bibliography 1 (" Study on Supermicro-pulverization of Traditional Chinese Drugs present Research and thinking ",
Zhao Ruizhi, 2013 biologic grain technologies of preparing and commercial application technical seminar) just record：Below 20 μm, reduce medicinal material
Particle size is little to the effect of anthraquinone dissolution in increase rheum officinale；For safflower and the root bark of tree peony, ultramicro grinding can not increase
The stripping quantity of main component；Although ultramicro grinding ginseng can increase the stripping quantity of ginsenoside and polysaccharide, to curative effect without notable
Increasing action.In addition, Chinese medicine, after micronization, physicochemical property often changes, to medicine post-production and
Use increase difficulty.In addition, in addition to Chinese medicine self-characteristic, the energy of superfine communication technique, especially low temperature overtemperature crushing technology
Consumption is big, and of high cost is also one of problem for running into above-mentioned technology applied to Chinese medicine processing.
Therefore, in order to improve cell-wall breaking ratio, the dissolution of active principle is increased, it may be considered that broken using low-temperature submicron powder
Mode processes tendril-leaved fritillary bulb, but needs to solve following technical problem：(1) it is adapted to the broken process conditions of low-temperature submicron powder of tendril-leaved fritillary bulb；(2) crush
Before, easily there is browning in tendril-leaved fritillary bulb drying process；(3) after low-temperature submicron powder is broken, physicochemical property may occur tendril-leaved fritillary bulb
Change, be unfavorable for following process and utilization.
In view of this, it is special to propose the present invention.
The content of the invention
The first object of the present invention is to provide a kind of method for processing tendril-leaved fritillary bulb, tendril-leaved fritillary bulb can be promoted to live by the method
The dissolution of property drug ingedient alkaloid and saponin(e.
The second object of the present invention is to provide a kind of tendril-leaved fritillary bulb preparation being prepared according to the above method, the preparation tool
The features such as active content of material is high, easy dissolution.
To solve the above problems, the present invention provides a kind of method for processing tendril-leaved fritillary bulb, the described method comprises the following steps：
(1), by tendril-leaved fritillary bulb section or coarse crushing, afterwards add rosa bella fruit ethanol extract, at room temperature soak 1~
2h, the addition of the ethanol extract of the rosa bella fruit are not have the tendril-leaved fritillary bulb at least；
(2), tendril-leaved fritillary bulb is dried to its water content at 70~100 DEG C and is less than 8%；
(3), the dried tendril-leaved fritillary bulb of ultramicro grinding at -35~-25 DEG C, the particle diameter to more than 95% tendril-leaved fritillary bulb ultra-micro powder exist
In the range of 400~600 mesh.
First, the present invention is using the broken technology processing tendril-leaved fritillary bulb of low-temperature submicron powder, and probes into thin in different temperatures and different crushing
Under degree, the stripping quantity and drug effect of active pharmaceutical ingredient in tendril-leaved fritillary bulb ultra-micro powder.According to present specification experimental example 1~2
Experimental data understand, by tendril-leaved fritillary bulb crush the meticulous dissolution that can not be effectively increased active material and lifting tendril-leaved fritillary bulb the effect of,
This is probably that the electric charge and adhesion on powder surface etc. change since tendril-leaved fritillary bulb is ground meticulous, although particle diameter smaller,
It is unfavorable for the release of active ingredient on the contrary.In addition, tendril-leaved fritillary bulb, during low-temperature submicron powder is broken, temperature is lower, active ingredient it is molten
Extracting rate is higher, but after temperature is less than -35 DEG C, with the reduction of temperature, the increase of total alkaloid and total saposins dissolution rate is simultaneously
Unobvious.Therefore, the dissolution rate of active ingredient, therapeutic efficiency and processing cost (temperature in tendril-leaved fritillary bulb ultra-micro powder is considered
Lower, powder the particle diameter of degree is smaller, and processing cost is about high) after, the optimised process bar of the broken tendril-leaved fritillary bulb of final definite low-temperature submicron powder
Part is：The dried tendril-leaved fritillary bulb of ultramicro grinding at -25~-35 DEG C, to more than 95% tendril-leaved fritillary bulb ultra-micro powder particle diameter 400~
In the range of 600 mesh.
Secondly, it is the brittleness of increase material, reduces the difficulty of crushing, before the crushing of low temperature overtemperature, is typically necessary pair
Processing is dried in material, reduces the water content of material.Due to the instrument that processing method is simple, need not be complicated, high-temperature heating
Drying is common drying mode.The present invention can rapidly obtain that degree of drying is good, water content using the mode of high temperature drying
Low tendril-leaved fritillary bulb, but in the heat drying process, brown stain easily occurs for tendril-leaved fritillary bulb, and the content of alkaloid is reduced, tendril-leaved fritillary bulb quality decline.
To overcome the defect, applicant takes multitude of different ways to pre-process tendril-leaved fritillary bulb, including using Vc,
NaHSO3, citric acid, Puerarin, resveratrol, the ethanol extract etc. of the ethanol extract of buckwheat seed and rosa bella fruit exist
Interior a variety for the treatment of fluids carry out immersion treatment to tendril-leaved fritillary bulb, to reduce the browning of tendril-leaved fritillary bulb in the drying process.This final hair
It is bright surprisingly it has been found that with Vc, NaHSO3, citric acid, the processing liquid phase ratio such as ethanol extract of Puerarin and buckwheat seed,
After ethanol extract immersion treatment by rosa bella fruit, browning of the tendril-leaved fritillary bulb in high-temperature drying procedures significantly reduces, always
The decline of alkaloid is also significantly inhibited.Effect of the ethanol extract of rosa bella fruit in terms of tendril-leaved fritillary bulb browning is suppressed with
Resveratrol treatment fluid is substantially suitable, but the former can largely be prepared using rosa bella fruit as raw material by simply leaching step,
It is easy to operate and of low cost, and resveratrol needs to isolate and purify and can obtain by complicated.At present, the second of rosa bella fruit
Alcohol extract can suppress the specific raw material of tendril-leaved fritillary bulb browning as caused by high temperature drying and be still not clear.But regardless of rosa bella fruit
How ethanol extract specifically plays a role, its inhibition to tendril-leaved fritillary bulb browning is unquestionable.
In conclusion the above method of the present invention is used before heat drying described in the ethanol extract processing of rosa bella fruit
Tendril-leaved fritillary bulb, not only contains that the effect of tendril-leaved fritillary bulb browning is good, and cost is low, cost-effective.
In some embodiments, the ethanol extract of the rosa bella fruit extracts in the following manner：By rosa bella fruit
Section, drying simultaneously crush, and afterwards, rosa bella fruit, separation of solid and liquid, through activated carbon decolorizing, up to the mountain are extracted with ethanol solution
The ethanol extract of rose hip.
In some embodiments, the ethanol extract of the rosa bella fruit is extracted especially by the following manner：Mountain is pierced
Rose fruit is cut into slices, and at 70~100 DEG C it is dry 12~24 it is small when, afterwards, crush the rosa bella fruit, cross 50~100 mesh sieves, press
10~15g of mass volume ratio:The ratio of 100mL adds the ethanol solution of 60~95% volume fractions, when extraction 2~4 is small, solid-liquid
Separation, adds the activated carbon of 1~5% mass fraction, shakes 20~40min, filtering, up to the ethanol extract of rosa bella fruit.
In some embodiments, between step (2) and step (3), the method is further comprising the steps of：By tendril-leaved fritillary bulb
Crush, cross 50~100 mesh sieves, be dissolved in water into tendril-leaved fritillary bulb slurry, afterwards, high-pressure homogeneous processing is carried out to slurry, after processing
Slurry carries out frozen drying.
Add water to cook be tendril-leaved fritillary bulb medicine materical crude slice conventional treatment method, can further promote alkaloid and saponin(e by decocting
Release.But invention it has been surprisingly found that compared with directly taking after mixing it with water or soaking using hot water, by the broken place of low-temperature submicron powder
The tendril-leaved fritillary bulb ultra-micro powder of reason can not increase the release of alkaloid and saponin(e, the dissolution of opposite alkaloid and saponin(e after decoction
Amount is reduced, and can be effectively increased pan-fried to avoid this phenomenon if carrying out high-pressure homogeneous operation to tendril-leaved fritillary bulb before ultramicro grinding
During boiling, the burst size of alkaloid and saponin(e.
At present, it is still not clear for the producing cause of this phenomenon, it may be possible to since the particle diameter of tendril-leaved fritillary bulb ultra-micro powder is meticulous,
Starch or protein is gelatinized in decoction process, be unfavorable for the leaching of active principle, and the high pressure before ultramicro grinding
Homogeneous operation makes starch in tendril-leaved fritillary bulb and protein-modified, and the gelatinization under high temperature is suppressed, thus increase alkaloid and
The burst size of saponin(e.
In some embodiments, the concrete mode of the high-pressure homogeneous processing includes：Under the pressure of 20~30MPa
Homogenization 1~2 minute.
In some embodiments, the method is further comprising the steps of：Added into tendril-leaved fritillary bulb ultra-micro powder and account for its weight
30%~50% ethanol solution, stirs evenly, and softwood, granulation, dried and screened are made, up to tendril-leaved fritillary bulb particle, the ethanol
The volume fraction of ethanol is 60~80% in solution.The above method of the present invention does not add any excipient in pelletization, no
But the Chinese medicine possessed all natural characteristic, and preparation process is very simple in itself can be effectively kept, is easily formed
Industrialized production.
In some embodiments, the method is further comprising the steps of：Tendril-leaved fritillary bulb ultra-micro powder is uniformly mixed with auxiliary material
Afterwards, it is tabletted；Preferably, the auxiliary material includes microcrystalline cellulose, pregelatinized starch, lactose, carboxymethyl starch, phosphoric acid hydrogen
One or more in calcium, gas phase superfine silica gel powder, magnesium stearate.
In some embodiments, the method is further comprising the steps of：By 10~15g of mass volume ratio:100mL's
Ratio adds the ethanol solution of 60~95% volume fractions in tendril-leaved fritillary bulb ultra-micro powder, when extraction 1~3 is small, separation of solid and liquid, and gained
Supernatant, that is, tendril-leaved fritillary bulb extracting solution.
In some embodiments, the tendril-leaved fritillary bulb is selected from bulbus fritillariae cirrhosae F.cirrhosa D.Don, Fritillaria unibracteata
F.unibracteata Hsiao et K.C.Hsia, Gansu fritillaria F.przewalskii Maxim. and Bulbus Fritillariae cirrhosae
One or more in F.delavayi Franch, it is preferable that the tendril-leaved fritillary bulb is bulbus fritillariae cirrhosae F.cirrhosa D.Don.
The present invention also provides the tendril-leaved fritillary bulb preparation being prepared according to the above method.The above-mentioned tendril-leaved fritillary bulb preparation of the present invention has cell
Sporoderm-broken rate is high, active ingredient dissolution rate is high, the advantages of can directly taking after mixing it with water, soak or decoct.
Compared with prior art, beneficial effects of the present invention are：
1), the present invention finally determines after active principle stripping quantity, drug effect and the cost of tendril-leaved fritillary bulb ultra-micro powder is considered
The broken optimum process condition of tendril-leaved fritillary bulb low-temperature submicron powder：The dried tendril-leaved fritillary bulb of ultramicro grinding at -35~-25 DEG C, to more than 95%
The particle diameter of tendril-leaved fritillary bulb ultra-micro powder is in the range of 400~600 mesh.At the process conditions, not only the alkaloid of tendril-leaved fritillary bulb and saponin(e are molten
Output increase, drug effect lifting, and have the advantages that energy saving, cost is low and cost-effective.
2), the method for the invention soaks tendril-leaved fritillary bulb using the ethanol extract of rosa bella fruit before high temperature drying
Processing, can effectively suppress the melting brown rate of tendril-leaved fritillary bulb in high-temperature drying procedures, reduce the loss of alkaloid.
3), the method for the invention carries out high-pressure homogeneous processing before low-temperature submicron powder is broken to tendril-leaved fritillary bulb, by the processing
It can solve tendril-leaved fritillary bulb ultra-micro powder alkaloid and the defects of not high saponin(e dissolution rate in decoction process.
4), tendril-leaved fritillary bulb preparation of the present invention has cell-wall breaking ratio height, active ingredient dissolution rate high, can directly take after mixing it with water, soak
The advantages of bubble or decoction.
Embodiment
Embodiment of the present invention is described in detail below in conjunction with embodiment, but those skilled in the art will
Understand, the following example is merely to illustrate the present invention, and is not construed as limiting the scope of the invention.It is not specified in embodiment specific
Condition person, the condition suggested according to normal condition or manufacturer carry out.Reagents or instruments used without specified manufacturer, is
The conventional products that can be obtained by commercially available purchase.
Embodiment 1
Tendril-leaved fritillary bulb is processed by the following method：
1st, net system：Qualified fresh tendril-leaved fritillary bulb Chinese medicine (bulbus fritillariae cirrhosae F.cirrhosa D.Don) will be examined, remove impurity, wash
Only, dry.
2nd, by tendril-leaved fritillary bulb sabot, it is 8% or so to be put into drying machine drying to its water content at 70 DEG C, afterwards, is stopped dry
It is dry, it is cooled to room temperature.
3rd, coarse crushing is carried out to dried tendril-leaved fritillary bulb piece using multifunctional crusher, obtains the tendril-leaved fritillary bulb coarse powder that particle diameter is 50 mesh.
4th, ultramicro grinding is carried out to tendril-leaved fritillary bulb coarse powder at -30 DEG C with the broken machine of oscillatory type low-temperature submicron powder, be crushed to 95% with
The particle diameter of upper tendril-leaved fritillary bulb ultra-micro powder is about 500 mesh.
5th, tendril-leaved fritillary bulb ultra-micro powder is uniformly mixed, afterwards, adds the ethanol solution of 60% volumetric concentration as adhesive, with
Tendril-leaved fritillary bulb ultra-micro powder stirs evenly, and softwood is made, and is pelletized by granulator, is dried at 60 DEG C to moisture content and is less than 5%, with 24 mesh
Sieve whole grain, obtains the conforming particle for meeting granularity requirements, the mass ratio of the tendril-leaved fritillary bulb ultra-micro powder and ethanol solution is 70:
30。
6th, above-mentioned tendril-leaved fritillary bulb particle is always uniformly mixed, is less than the difference of each sample point particulate samples of same batch products
3%.
7th, qualified tendril-leaved fritillary bulb particle will be examined to be dispensed with infusion packet by 3g/ bags.
Embodiment 2
Tendril-leaved fritillary bulb is processed by 1 the method for embodiment, is differed only in, the grain of more than 95% tendril-leaved fritillary bulb ultra-micro powder in step 4
Footpath is about 400 mesh.
Embodiment 3
Tendril-leaved fritillary bulb is processed by 1 the method for embodiment, is differed only in, the grain of more than 95% tendril-leaved fritillary bulb ultra-micro powder in step 4
Footpath is about 600 mesh.
Embodiment 4
Tendril-leaved fritillary bulb is processed by 1 the method for embodiment, is differed only in, the temperature in step 4 during ultramicro grinding is -25 DEG C.
Embodiment 5
Tendril-leaved fritillary bulb is processed by 1 the method for embodiment, is differed only in, the temperature in step 4 during ultramicro grinding is -35 DEG C.
Embodiment 6
Tendril-leaved fritillary bulb is processed by the following method：
1st, net system：Qualified fresh tendril-leaved fritillary bulb Chinese medicine (bulbus fritillariae cirrhosae F.cirrhosa D.Don) will be examined, remove impurity, wash
Only, dry.
2nd, cut into slices using slicer to tendril-leaved fritillary bulb, obtain the homogeneous tendril-leaved fritillary bulb piece of thickness.
3rd, the ethanol extract of rosa bella fruit is prepared：Rosa bella fruit is cut into slices, dry 12h is placed at 70 DEG C, after drying
Sample with multifunctional sample pulverizer crush after cross 80 mesh sieves, by mass volume ratio 1g:The ratio of 10mL adds 75% ethanol
Solution, when extraction 3 is small, separation of solid and liquid, adds the activated carbon of 5% mass fraction, shakes 30min, filtering, is pierced up to mountain afterwards
The ethanol extract of rose fruit.
4th, the ethanol extract of rosa bella fruit is added in tendril-leaved fritillary bulb piece, soaks tendril-leaved fritillary bulb piece at room temperature 30 minutes, wherein
The addition of ethanol extract is advisable with not crossing tendril-leaved fritillary bulb piece.
5th, after treatment, tendril-leaved fritillary bulb piece is dried, sabot, is put into drying machine drying to its water content at 70 DEG C and is
5% or so, afterwards, stop drying, be cooled to room temperature.
6th, coarse crushing is carried out to dried tendril-leaved fritillary bulb piece using multifunctional crusher, obtains the tendril-leaved fritillary bulb coarse powder that particle diameter is 50 mesh.
7th, ultramicro grinding is carried out to tendril-leaved fritillary bulb coarse powder at -30 DEG C with the broken machine of oscillatory type low-temperature submicron powder, tendril-leaved fritillary bulb surpasses after crushing
The average fineness of fine powder is about 500 mesh.
8th, tendril-leaved fritillary bulb ultra-micro powder is uniformly mixed, afterwards, adds the ethanol solution of 70% volumetric concentration as adhesive, with
Tendril-leaved fritillary bulb ultra-micro powder stirs evenly, and softwood is made, and is pelletized by granulator, is dried at 60 DEG C to moisture content and is less than 5%, with 24 mesh
Sieve whole grain, obtains the conforming particle for meeting granularity requirements, the mass ratio of the tendril-leaved fritillary bulb ultra-micro powder and ethanol solution is 70:
30。
9th, above-mentioned tendril-leaved fritillary bulb particle is always uniformly mixed, is less than the difference of each sample point particulate samples of same batch products
3%.
10th, qualified tendril-leaved fritillary bulb particle will be examined to be dispensed with immersion band by 3g/ bags.
Embodiment 7
Tendril-leaved fritillary bulb is processed by the following method：
1st, net system：Qualified fresh tendril-leaved fritillary bulb Chinese medicine (bulbus fritillariae cirrhosae F.cirrhosa D.Don) will be examined, remove impurity, wash
Only, dry.
2nd, cut into slices using slicer to tendril-leaved fritillary bulb, obtain the homogeneous tendril-leaved fritillary bulb piece of thickness.
3rd, the ethanol extract of rosa bella fruit is prepared：Rosa bella fruit is cut into slices, dry 24h is placed at 70 DEG C, after drying
Sample with multifunctional sample pulverizer crush after cross 50 mesh sieves, by mass volume ratio 1g:The ratio of 10mL adds 75% ethanol
Solution, when extraction 3 is small, separation of solid and liquid, adds the activated carbon of 5% mass fraction, shakes 30min, filtering, is pierced up to mountain afterwards
The ethanol extract of rose fruit.
4th, the ethanol extract of rosa bella fruit is added in tendril-leaved fritillary bulb piece, soaks tendril-leaved fritillary bulb piece at room temperature 30 minutes, wherein
The addition of ethanol extract is advisable with not crossing tendril-leaved fritillary bulb piece.
5th, after treatment, tendril-leaved fritillary bulb piece is dried, sabot, is put into drying machine drying to its water content at 70 DEG C and is
5% or so, afterwards, stop drying, be cooled to room temperature.
6th, coarse crushing is carried out to dried tendril-leaved fritillary bulb piece using multifunctional crusher, obtains the tendril-leaved fritillary bulb coarse powder that particle diameter is 50 mesh.
7th, the tendril-leaved fritillary bulb coarse powder water of 3 times of volumes is dissolved, defibrination, obtains tendril-leaved fritillary bulb slurry, pressed afterwards with homogenizer in 30MPa
Homogenization 2 minutes under power.
8th, the slurry Jing Guo high-pressure homogeneous processing is freeze-dried, the condition of freeze-drying is dry at -40 DEG C
36h。
9th, the powder agglomates obtained with the broken machine of oscillatory type low-temperature submicron powder at -30 DEG C to freeze-drying carries out ultramicro grinding, powder
The average fineness of tendril-leaved fritillary bulb micropowders is about 500 mesh after broken.
10th, tendril-leaved fritillary bulb ultra-micro powder is uniformly mixed, afterwards, adds the ethanol solution of 80% volumetric concentration as adhesive,
Stirred evenly with tendril-leaved fritillary bulb ultra-micro powder, softwood is made, pelletized by granulator, dried at 70 DEG C to moisture content and be less than 5%, with
24 mesh sieve net whole grains, obtain the conforming particle for meeting granularity requirements, and the mass ratio of the tendril-leaved fritillary bulb ultra-micro powder and ethanol solution is
80:20。
11st, above-mentioned tendril-leaved fritillary bulb particle is always uniformly mixed, is less than the difference of each sample point particulate samples of same batch products
3%.
12nd, qualified tendril-leaved fritillary bulb particle will be examined to be dispensed with immersion band by 3g/ bags.
Embodiment 8
With reference to 7 the method for embodiment processing tendril-leaved fritillary bulb, it is differed only in, and the pressure of high homogenization is in step 7
20MPa。
Embodiment 9
With reference to 7 the method for embodiment processing tendril-leaved fritillary bulb, it is differed only in, and the pressure of step 7 mesohigh homogenization is
25MPa。
Comparative example 1
Tendril-leaved fritillary bulb is processed by the following method：
1st, net system：Qualified fresh tendril-leaved fritillary bulb Chinese medicine (bulbus fritillariae cirrhosae F.cirrhosa D.Don) will be examined, remove impurity, wash
Only, dry.
2nd, by tendril-leaved fritillary bulb sabot, it is 8% or so to be put into drying machine drying to its water content at 70 DEG C, afterwards, is stopped dry
It is dry, it is cooled to room temperature.
3rd, coarse crushing is carried out to dried tendril-leaved fritillary bulb piece using multifunctional crusher, obtains the tendril-leaved fritillary bulb coarse powder that particle diameter is 50 mesh.
4th, tendril-leaved fritillary bulb ultra-micro powder is uniformly mixed, afterwards, adds the ethanol solution of 60% volumetric concentration as adhesive, with
Tendril-leaved fritillary bulb ultra-micro powder stirs evenly, and softwood is made, and is pelletized by granulator, is dried at 70 DEG C to moisture content and is less than 5%, with 24 mesh
Sieve whole grain, obtains the conforming particle for meeting granularity requirements, the mass ratio of the tendril-leaved fritillary bulb ultra-micro powder and ethanol solution is 60:
40。
5th, above-mentioned tendril-leaved fritillary bulb particle is always uniformly mixed, is less than the difference of each sample point particulate samples of same batch products
3%.
6th, qualified tendril-leaved fritillary bulb particle will be examined to be dispensed with immersion band by 3g/ bags.
Comparative example 2~8
Comparative example 2~8 is with reference to 1 the method for embodiment processing tendril-leaved fritillary bulb, it is differed only in, more than 95% river in step 4
The particle diameter of shellfish ultra-micro powder respectively may be about 100 mesh, 200 mesh, 300 mesh, 700 mesh, 800 mesh, 900 mesh and 1000 mesh.
Comparative example 9~14
Comparative example 9~14 is with reference to 1 the method for embodiment processing tendril-leaved fritillary bulb, it is differed only in, low temperature ultra micro in step 4
The temperature of crushing is respectively -10 DEG C, -15 DEG C, -20 DEG C, -40 DEG C, -45 DEG C and -50 DEG C.
Comparative example 15~20
Comparative example 15~20 is with reference to 6 the method for embodiment processing tendril-leaved fritillary bulb, it is differed only in, and step 3-4 is：With
0.1M phosphate-buffereds prepare Vc treatment fluids (0.1g/L), NaHSO respectively3Treatment fluid (0.2g/L), citric acid treatment liquid (15g/
L), the ethanol extract of Puerarin treatment fluid (0.001mol/L), resveratrol treatment fluid (0.1mol/L) and buckwheat seed, will
Above-mentioned treatment fluid is added in the tendril-leaved fritillary bulb piece, is advisable with excessively not described tendril-leaved fritillary bulb piece, is handled 30 minutes.The wherein second of buckwheat seed
Alcohol extract obtains in the following manner：Buckwheat seed is removed the peel, when drying 12 is small at 80 DEG C, 80 mesh sieves is crossed after crushing, are pressed
Mass volume ratio 10g：The ratio of 100ml is added in 60% ethanol solution, when extraction 3 is small, separation of solid and liquid, up to buckwheat
The ethanol extract of son.
Comparative example 21~24
Comparative example 21~24 processes tendril-leaved fritillary bulb with reference to 7 the method for embodiment, differs only in, step 7 mesohigh homogeneous
Processing pressure is respectively 10MPa, 40MPa, 50MPa and 60MPa.
Experimental example 1
Detect embodiment 1~5 and the stripping quantity of total alkaloid and total saposins in the tendril-leaved fritillary bulb particle of comparative example 1~14, tool
Body testing result is the stripping quantity of total alkaloid and total saposins in tendril-leaved fritillary bulb particle under different-grain diameter referring to Tables 1 and 2, wherein table 1,
Table 2 is total alkaloid and the content of total saposins in tendril-leaved fritillary bulb particle under different temperatures.
The specific detection method of total alkaloid stripping quantity is as follows：Take 5g tendril-leaved fritillary bulb particles, water logging is drunk with 100mL, 70 DEG C
15min is steeped, separation of solid and liquid, the liquid of acquisition is evaporated in water-bath afterwards, and residue is dissolved with a small amount of chloroform, then is evaporated,
Residue adds 10ml ether dissolutions, adds the standard sulfuric acid solution of 10ml 0.001mol/L, and ether is carefully removed in water-bath, is added
15ml newly boils the distilled water of cooling, makees indicator with methyl red, and with 0.002mol/L standard caustic soda solution residual titrations, titration is eventually
Point solution is yellow by red change.Alkaloid calculates as follows：
The molar concentration of total alkaloid percentage composition=2MVm100%/(1000W), wherein M- standards sulfuric acid solution, V- leachings
The milliliter number of consumption standard sulfuric acid solution, W- sample grams, the molecular weight of m- fritimines (in terms of imperialine, 429).
The specific detection of total saposins stripping quantity is as follows：5g tendril-leaved fritillary bulb ultra-micro powders are taken, are soaked with 100mL, 70 DEG C of drinking water
15min, separation of solid and liquid, the liquid of acquisition is evaporated in water-bath afterwards, and residue 20mL methanol dissolves, and adds ether 50ml,
Mix, stood overnight in refrigerator, topple over supernatant, precipitation uses ether 10mL, is dissolved by heating after washing with 30mL methanol, with through dry
The dry incipient fusion glass hourglass bucket to constant weight filters, and filtrate adds ether 50mL, stood overnight in refrigerator, is filtered with incipient fusion glass hourglass bucket
Cross, drain, be dried under vacuum to constant weight in 60 DEG C, weigh, subtract funnel weight, obtain the content of total saposins in sample, and calculate sample
The mass fraction of total saposins in product.
The stripping quantity of total alkaloid and total saposins in tendril-leaved fritillary bulb particle under table 1- different-grain diameters
The stripping quantity of total alkaloid and total saposins in tendril-leaved fritillary bulb particle at a temperature of the different crushing of table 2-
Experimental example 2
Detect embodiment 1~5 and the antitussive effect and phlegm-dispelling functions of the tendril-leaved fritillary bulb particle of comparative example 1~14：
1st, cavy citric acid draws cough experiment
The cavy of 200 ± 50g or so is equally divided into 20 groups, every group 3, correspond to respectively blank control group, embodiment 1~
5 and comparative example 1~14.Example 1~5 and tendril-leaved fritillary bulb particle 1g of comparative example 1~14, adds 5mL water, and tendril-leaved fritillary bulb suspension is made
Liquid, gavage is carried out to mouse, by 3 times/day, common gavage 5 days, wherein using drinking water as blank control, to control group mice
Carry out gavage.After administration in the 5th day terminates 1h, sprayed with 17.5% citric acid stimulates each group, after 30s, observes and records
The cough number of cavy in 5min (specific testing result is referring to table 3).
2nd, the expectoration of rat capillary is tested
SD rats are randomly divided into 20 groups, every group 3, correspond to blank control group, embodiment 1~5 and comparative example 1 respectively
~14.Example 1~5 and the tendril-leaved fritillary bulb particle 1g of comparative example 1~14, add 5mL water, the micro- suspension of tendril-leaved fritillary bulb are made, to rat into
Row gavage, by 3 times/day, common gavage 5 days, after the 5th day is administered 1h, 25% urethane is anaesthetized by 1g/kg, and back of the body position is fixed, exposure gas
Pipe, the 3rd ring cartilage ring position is inserted into diameter 0.5mm capillary glass tubies under thyroid cartilage ring, the sputum of 2h is collected, with 2h
The length of each group sputum and quality of sputum is analyzed (specific testing result is referring to table 3) for index in the unit interval.
The cough-relieving of table 3- tendril-leaved fritillary bulb particles and town asthma effect
Experimental example 3
1st, detect 15~19 high temperature drying of embodiment 1,6 and comparative example after tendril-leaved fritillary bulb brown stain degree：Take dry front and rear tendril-leaved fritillary bulb
Piece 1g wears into homogenate, adds 10ml distilled water, is settled at centrifuge tube maximum capacity, and 4000rpm centrifugation 20min, take supernatant
It is spare.Using light absorption value method, light absorption value, brown stain degree=OD460 are measured at 460nm on ultraviolet specrophotometerBefore drying-
OD460After drying, specific testing result is referring to table 5.
2nd, total alkaloid and the content of saponin(e in leachate are detected：15~19 tendril-leaved fritillary bulb of Example 1,6 and comparative example
Particle 5g, adds the warm water of 70 DEG C of 100ml, soaks 15 minutes, separation of solid and liquid, detects the molten of total alkaloid and saponin(e in leachate
Output, specific detection method is referring to experimental example 1, and specific testing result is referring to table 4.
The detection of table 4- tendril-leaved fritillary bulb brown stain degree and active material dissolution rate
Experimental example 4
Example 1,7-9 and the tendril-leaved fritillary bulb particle of comparative example 20~23,5g, add 150mL water, decoct 10 minutes, solid-liquid
Separation, detects the stripping quantity of total alkaloid and total saposins in decoction liquor, specific detection method is referring to experimental example 1, specific detection knot
Fruit is referring to table 5.
The stripping quantity of total alkaloid and total saposins in tendril-leaved fritillary bulb particle in table 5- decoction liquors
Finally it should be noted that：The above embodiments are only used to illustrate the technical solution of the present invention., rather than its limitations；To the greatest extent
Pipe is described in detail the present invention with reference to foregoing embodiments, but it will be understood by those of ordinary skill in the art that：Its
It can still modify to the technical solution described in foregoing embodiments, either to which part or all technical characteristic
Carry out equivalent substitution；And these modifications or replacement, the essence of appropriate technical solution is departed from various embodiments of the present invention skill
The scope of art scheme.
Claims (10)
- A kind of 1. method for processing tendril-leaved fritillary bulb, it is characterised in that the described method comprises the following steps：(1), by tendril-leaved fritillary bulb section or coarse crushing, the ethanol extract of rosa bella fruit is added afterwards, soaks 1~2h, institute at room temperature The addition for stating the ethanol extract of rosa bella fruit is not have the tendril-leaved fritillary bulb at least；(2), tendril-leaved fritillary bulb is dried to its water content at 70~100 DEG C and is less than 8%；(3), the dried tendril-leaved fritillary bulb of ultramicro grinding at -35~-25 DEG C, to more than 95% tendril-leaved fritillary bulb ultra-micro powder particle diameter 400 In the range of~600 mesh.
- 2. according to the method described in claim 1, it is characterized in that, the ethanol extract of the rosa bella fruit in the following manner Extraction：Rosa bella fruit is cut into slices, dries and crushes, afterwards, rosa bella fruit, separation of solid and liquid, through activated carbon are extracted with ethanol solution Decoloration, up to the ethanol extract of the rosa bella fruit.
- 3. according to the method described in claim 2, it is characterized in that, the ethanol extract of the rosa bella fruit is especially by following Mode is extracted：Rosa bella fruit is cut into slices, at 70~100 DEG C it is dry 12~24 it is small when, afterwards, crush the rosa bella fruit, cross 50~ 100 mesh sieves, by 10~15g of mass volume ratio:The ethanol solution of ratio 60~95% volume fractions of addition of 100mL, extraction 2~ 4 it is small when, separation of solid and liquid, add 1~5% mass fraction activated carbon, shake 20~40min, filtering, up to the second of rosa bella fruit Alcohol extract.
- 4. according to the method described in claim 1, it is characterized in that, between step (2) and step (3), the method is also wrapped Include following steps：Tendril-leaved fritillary bulb is crushed, 50~100 mesh sieves is crossed, is dissolved in water into tendril-leaved fritillary bulb slurry, it is afterwards, equal into horizontal high voltage to slurry Matter processing, frozen drying is carried out by the slurry after processing.
- 5. according to the method described in claim 4, it is characterized in that, the concrete mode of the high-pressure homogeneous processing includes：20 Homogenization 1~2 minute under the pressure of~30MPa.
- 6. according to claim 1-5 any one of them methods, it is characterised in that the method is further comprising the steps of：Xiang Chuan The ethanol solution for accounting for its weight 30%~50% is added in shellfish ultra-micro powder, stirs evenly, softwood, granulation, drying and mistake is made Sieve, up to tendril-leaved fritillary bulb particle, the volume fraction of ethanol is 60~80% in the ethanol solution.
- 7. according to claim 1-5 any one of them methods, it is characterised in that the method is further comprising the steps of：By river Shellfish ultra-micro powder and auxiliary material are after mixing, tabletted；Preferably, the auxiliary material includes microcrystalline cellulose, pregelatinated forms sediment One or more in powder, lactose, carboxymethyl starch, calcium monohydrogen phosphate, gas phase superfine silica gel powder, magnesium stearate.
- 8. according to claim 1-5 any one of them methods, it is characterised in that the method is further comprising the steps of：By matter Measure 10~15g of volume ratio:The ratio of 100mL adds the ethanol solution of 60~95% volume fractions in tendril-leaved fritillary bulb ultra-micro powder, leaching Carry 1~3 it is small when, separation of solid and liquid, gained supernatant is tendril-leaved fritillary bulb extracting solution.
- 9. according to claim 1-5 any one of them methods, it is characterised in that the tendril-leaved fritillary bulb is selected from bulbus fritillariae cirrhosae F.cirrhosa D.Don, Fritillaria unibracteata F.unibracteata Hsiao et K.C.Hsia, Gansu fritillaria F.przewalskii Maxim. and One or more in Bulbus Fritillariae cirrhosae F.delavayi Franch, it is preferable that the tendril-leaved fritillary bulb is bulbus fritillariae cirrhosae F.cirrhosa D.Don。
- 10. tendril-leaved fritillary bulb preparation is prepared according to any one of claim 1-9 the method.
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| CN110249947A (en) * | 2019-07-15 | 2019-09-20 | 丽江绿之源生物药业科技开发有限公司 | A kind of method for culturing seedlings of Bulbus Fritillariae cirrhosae |
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| CN110249947A (en) * | 2019-07-15 | 2019-09-20 | 丽江绿之源生物药业科技开发有限公司 | A kind of method for culturing seedlings of Bulbus Fritillariae cirrhosae |
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