CN106880737A - A kind of preparation method of taipei fritillary bulb ultra micro freeze-dried powder - Google Patents
A kind of preparation method of taipei fritillary bulb ultra micro freeze-dried powder Download PDFInfo
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- CN106880737A CN106880737A CN201510942235.7A CN201510942235A CN106880737A CN 106880737 A CN106880737 A CN 106880737A CN 201510942235 A CN201510942235 A CN 201510942235A CN 106880737 A CN106880737 A CN 106880737A
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K36/00—Medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicines
- A61K36/18—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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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K9/00—Medicinal preparations characterised by special physical form
- A61K9/14—Particulate form, e.g. powders, Processes for size reducing of pure drugs or the resulting products, Pure drug nanoparticles
- A61K9/19—Particulate form, e.g. powders, Processes for size reducing of pure drugs or the resulting products, Pure drug nanoparticles lyophilised, i.e. freeze-dried, solutions or dispersions
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2236/00—Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
- A61K2236/10—Preparation or pretreatment of starting material
- A61K2236/15—Preparation or pretreatment of starting material involving mechanical treatment, e.g. chopping up, cutting or grinding
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2236/00—Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
- A61K2236/30—Extraction of the material
- A61K2236/31—Extraction of the material involving untreated material, e.g. fruit juice or sap obtained from fresh plants
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2236/00—Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
- A61K2236/50—Methods involving additional extraction steps
- A61K2236/53—Liquid-solid separation, e.g. centrifugation, sedimentation or crystallization
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Abstract
The invention belongs to herb powder grinding preparing technical field, disclose a kind of preparation method of taipei fritillary bulb ultra micro freeze-dried powder, the present invention is with the larger taipei fritillary bulb of cultivation technique maturation, yield as raw material, cleaned and crush by ultrasonic wave, mechanical jordaning, centrifugation point liquid, high pressure microjet homogeneous, a cold sterilization, obtain target product taipei fritillary bulb ultra micro freeze-dried powder after eventually passing freeze-drying or spray drying, sieving.The preparation method of taipei fritillary bulb ultra micro freeze-dried powder of the present invention helps to retain the various alkaloids in taipei fritillary bulb, and preparation method is simple, time-consuming short, suitable industrialized production, farthest remains TA composition and the active component in taipei fritillary bulb；Simultaneously, the present invention does not produce toxin and unknown material, easy to operate economical and effective using medicine after high pressure cold sterilization, strong sterilizing power, drug effect free of losses, sterilizing, and the taipei fritillary bulb ultra micro freeze-dried powder for preparing belongs to Nano grade product, facilitate its follow-up directly use and deep processing.
Description
Technical field
The invention belongs to herb powder grinding preparing technical field, it is related to a kind of preparation method of taipei fritillary bulb ultra micro freeze-dried powder.
Background technology
Taipei fritillary bulb, also known as too shellfish, sharp shellfish, Qin shellfish, are the dry bulb of liliaceous plant, cure mainly lung-heat type cough, and the few phlegm of dry cough, deficiency of Yin labor is coughed, and cough up sputum streaked with blood, and 5 Chinese Pharmacopoeia of version 6 one is loaded under bulbus fritillariae cirrhosae within 2010.Taipei fritillary bulb has long medication history on Hubei Wu Feng, Chongqing Wuxi, Ningxia Jingyuan, Gansu Zhang Xian and other places, and commonly using product as the place of bulbus fritillariae cirrhosae always is used as medicine.Recorded with the name of bulbus fritillariae cirrhosae, BULBUS FRITILLARIAE CIRRHOSAE and disk shellfish respectively in Sichuan Province's Chinese medicine standard 6 (enlarged edition in 1987) of local medicinal material standard 5,5 Gansu Province's Chinese medicine quality standards 6 and 5 Ningxia Chinese medicine standards 6 (1993).Go through " blue or green shellfish " and " loose shellfish " that the Chinese Pharmacopoeia 6 (1977 ~ 2005 years) of version 5 is recorded, its plant origin is bulbus fritillariae cirrhosae, Fritillaria unibracteata and Gansu fritillaria, but in actual production, wild taipei fritillary bulb commodity morphologically are difficult to distinguish with above-mentioned 3 kinds source fritillarias, and its bulb also makees commodity " blue or green shellfish " and " loose shellfish " uses.Further, since bulbus fritillariae cirrhosae wild resource tends to exhausted, artificial low altitude area introduces a fine variety that difficulty is larger, and extensive cultivation not yet succeeds so far, and taipei fritillary bulb cultivation technique is more ripe, and yield is big, suitable low altitude area cultivation.The experimental results show taipei fritillary bulb chemical composition, phytomorph and pharmacological action and bulbus fritillariae cirrhosae does not have notable difference, but not yet draw attention.
Prior art is when using this taste medicinal material of bulbus fritillariae cirrhosae, generally use when shine dry chip using or by its main active substances extract be prepared into health products, medicinal material is not made full use of, and the medical value and using effect that bulbus fritillariae cirrhosae is prepared into powder are more preferably, can to greatest extent retain more active components.Ultra-fine powder technology is a kind of new crushing technology grown up to adapt to modern technology requirements, material is after fine, with minimum volume, thus it is easily attached to the surface of other materials and the rapid diffusion inside infiltration to these materials, there is physically or chemically effect with the surface of other materials and form closely combination, obtain very curative effect.The features such as Ultramicro-powder is conducive to retaining bioactive ingredients, improves dissolution rate, the difference of the drug effect that reduction is formed by absorption of human body difference, improves drug effect, material-saving resource, it is adaptable to which herb resource is not wide, the Chinese medicine more than residue active ingredient.Many Chinese medicines can be carried out ultramicro grinding, as Chinese medicine Ultramicro-powder.Contained effective substance is compared with traditional Chinese medicine medicine materical crude slice, Chinese medicine preparation in ultra micro Chinese medicine, change on obvious molecular structure will not occur, the change of Chinese medicine attribute, pharmacodynamic properties and indication will not be caused, be that herbal medicine efficacy and stabilization provide basic guarantee.
Prior art：A kind of bulbus fritillariae cirrhosae ultra-fine powder preparation technology, patent publication No.：CN103536747A, September is authorized on the 23rd within 2015, using following technical scheme：A kind of bulbus fritillariae cirrhosae ultra-fine powder preparation technology, comprises the following steps：(1) sorting；(2) it is beaten：The microcrystalline cellulose powder of 10 ~ 20wt% of material quality is added after raw material bulbus fritillariae cirrhosae preliminary crushing, then the raw material is sufficiently mixed with the microcrystalline cellulose by the rotation of mixer batch can, obtain batch mixing；It is subsequently adding the water mashing of 0.7 ~ 0.8 times of batch mixing quality；(3) pre-freeze：The Tween 80 of 10 ~ 15wt% of grind slurries quality is added before pre-freeze and is sufficiently stirred for；(4) freeze-drying, it is desirable to which moisture control is in below 6wt%；(5) break micro mist and micro mist is broken into by oscillatory type ultramicro grinding grinding kneading machine, bulbus fritillariae cirrhosae Ultramicro-powder prepared by the inventive method can farthest retain the active component in bulbus fritillariae cirrhosae.But microcrystalline cellulose this component is with the addition of during the reprocessing of this preparation method, the purity of tendril-leaved fritillary bulb female powder is have impact on, and this material of microcrystalline cellulose is water insoluble, be that the later stage of tendril-leaved fritillary bulb female powder uses and takes and makes troubles；Meanwhile, bulbus fritillariae cirrhosae plantation technique is not mature enough, and no taipei fritillary bulb of originating is extensive；The long processing time of this kind of preparation technology, during may result in bulbus fritillariae cirrhosae and infected by bacterium and microorganism.
The content of the invention
It is an object of the invention to provide a kind of preparation method of taipei fritillary bulb ultra micro freeze-dried powder, with the big taipei fritillary bulb of cultivation technique maturation, yield as raw material, cleaned and crush by ultrasonic wave, mechanical jordaning, high-pressure homogeneous, cold sterilization, eventually pass the mode such as freeze-drying or spray drying sieving, retain the active component of taipei fritillary bulb to greatest extent, the preparation method time is short, do not destroy the composition of taipei fritillary bulb, using scope it is wide, be adapted to industrialized production.
To achieve these goals, the technical solution adopted in the present invention is：A kind of preparation method of taipei fritillary bulb ultra micro freeze-dried powder, comprises the following steps：
Step 1, takes and dries standby taipei fritillary bulb sample, and being put into supersonic wave cleaning machine carries out cleaning and preliminary dispersion is crushed；
Step 2, the ultrasonically treated gained mixed liquor of step 1 is filtered, and filter cake and filter residue are used for mechanical jordaning, and filtrate carries out mechanical jordaning, taipei fritillary bulb slurries are obtained after mechanical jordaning with filter cake filter residue in the lump after sand core funnel filters off moisture to residual volume；
Step 3, the taipei fritillary bulb slurries to being obtained in step 2 carry out centrifugation point liquid, lower sediment thing and carry out homogeneous using high pressure microjet mode first, and supernatant is used for taipei fritillary bulb ultrasonic cleaning and dispersion in being recycled to step 1；
Step 4, the taipei fritillary bulb homogeneous solution obtained to step 3 by cold sterilization mode carries out ultra-high pressure sterilization, make sample that physical chemistry and the biological effects such as enzyme inactivation, protein denaturation, starch gelatinization and bacteria inactivation rate are produced under high pressure as pressure matchmaker using water, so as to reach sterilizing and modified purpose；
Step 5, taipei fritillary bulb ultra micro freeze-dried powder is obtained after being dried the taipei fritillary bulb homogeneous solution after being sterilized in step 4, cross sieve classification.
Step 1 ultrasonication power described in a kind of preparation method of above-mentioned taipei fritillary bulb ultra micro freeze-dried powder is 200~600W, and 20 ~ 60min of batch process under room temperature condition, ultrasonically treated concentration is 30% ~ 60%.
A kind of preparation method of above-mentioned taipei fritillary bulb ultra micro freeze-dried powder, mechanical jordaning is carried out in the step 2 using PFI fiberizers, and defibrination revolution is 1500r/min, grinding clearance 0.2mm, defibrination time 10min, 25 ± 5 DEG C of defibrination temperature.
A kind of preparation method of above-mentioned taipei fritillary bulb ultra micro freeze-dried powder, the drying of taipei fritillary bulb powder uses -50 DEG C of vacuum freeze drying in the step 5, and drying time is 24h.
A kind of preparation method of above-mentioned taipei fritillary bulb ultra micro freeze-dried powder, the drying of taipei fritillary bulb powder uses spray drying, 60 ~ 80 DEG C of drying temperature, 4 ~ 5h of drying time in the step 5.
A kind of preparation method of above-mentioned taipei fritillary bulb ultra micro freeze-dried powder, dried taipei fritillary bulb powder obtains taipei fritillary bulb ultra micro freeze-dried powder after crossing the screen cloth of 800 mesh in the step 5.
A kind of preparation method of above-mentioned taipei fritillary bulb ultra micro freeze-dried powder, the moisture content of taipei fritillary bulb ultra micro freeze-dried powder prepared by methods described is less than 3%, and average grain diameter is below 5 μm.
Beneficial effects of the present invention：The present invention provides a kind of preparation method of taipei fritillary bulb ultra micro freeze-dried powder, help to retain the various alkaloids in taipei fritillary bulb, preparation method is simple, time-consuming short, suitable industrialized production, farthest remains TA composition and the active component in taipei fritillary bulb；Simultaneously, the present invention further carries out dispersion and fining using high pressure microjet homogeneous manner to the taipei fritillary bulb after mechanical jordaning, toxin and unknown material are not produced using medicine after high pressure cold sterilization, strong sterilizing power, drug effect free of losses, sterilizing, any toxic and side effect is not produced to operator, easy to operate economical and effective, further, taipei fritillary bulb ultra micro freeze-dried powder prepared by the present invention belongs to Nano grade product, facilitates it subsequently directly to use and reprocess.
Specific embodiment
Embodiments of the invention are elaborated below：The present embodiment is implemented under premised on technical solution of the present invention, gives detailed implementation method and specific operating process.It should be pointed out that to those skilled in the art, without departing from the inventive concept of the premise, can also make some variations and modifications, these belong to the scope of the present invention.
Embodiment 1
A kind of preparation method of taipei fritillary bulb ultra micro freeze-dried powder, comprises the following steps：
Step 1, takes and dries that standby taipei fritillary bulb sample is appropriate and appropriate water, and being put into supersonic wave cleaning machine carries out cleaning and preliminary dispersion is crushed, and ultrasonication power is 300W, and batch process 30min under room temperature condition, ultrasonically treated concentration is 50%.
Step 2, the ultrasonically treated gained mixed liquor of step 1 is filtered, filter cake and filter residue are used for mechanical jordaning, filtrate carries out mechanical jordaning with filter cake and filter residue by PFI fiberizers in the lump after sand core funnel filters off moisture to residual volume, taipei fritillary bulb slurries are obtained after mechanical jordaning, defibrination revolution is 1500r/min, grinding clearance 0.2mm, defibrination time 10min, 25 DEG C of defibrination temperature.
Step 3, the taipei fritillary bulb slurries to being obtained in step 2 carry out centrifugation point liquid, lower sediment thing and carry out homogeneous using high pressure microjet mode first, and taipei fritillary bulb ultrasonic cleaning and dispersion is used in supernatant circulating and recovering to step 1；
Step 4, the taipei fritillary bulb homogeneous solution obtained to step 3 by cold sterilization mode carries out ultra-high pressure sterilization, make sample that physical chemistry and the biological effects such as enzyme inactivation, protein denaturation, starch gelatinization and bacteria inactivation rate are produced under high pressure as pressure matchmaker using water, so as to reach sterilizing and modified purpose；
Step 5, the taipei fritillary bulb homogeneous solution after being sterilized in step 4 is dried, and the vacuum freeze drying of -50 DEG C of drying condition, drying time is 24h；Dry taipei fritillary bulb powder is crossed afterwards taipei fritillary bulb ultra micro freeze-dried powder is obtained after 800 eye mesh screens, resulting ultra micro freeze-dried powder moisture content is less than 3%, and average grain diameter belongs to Nano grade product below 5 μm, facilitates it subsequently directly to use and reprocess.
Embodiment 2
A kind of preparation method of taipei fritillary bulb ultra micro freeze-dried powder, comprises the following steps：
Step 1, takes and dries standby taipei fritillary bulb sample, and being put into supersonic wave cleaning machine carries out cleaning and preliminary dispersion is crushed, and ultrasonication power is 200W, and batch process 20min under room temperature condition, ultrasonically treated concentration is 60%；
Step 2, the ultrasonically treated gained mixed liquor of step 1 is filtered, filter cake and filter residue are used for mechanical jordaning, filtrate is latter to residual volume by sand core funnel elimination moisture and carries out mechanical jordaning, and taipei fritillary bulb slurries are obtained after mechanical jordaning, and mechanical jordaning equipment is PFI fiberizers, defibrination revolution is 1500r/min, grinding clearance 0.2mm, defibrination time 10min, 25 ± 5 DEG C of defibrination temperature.
Step 3, the taipei fritillary bulb slurries to being obtained in step 2 carry out centrifugation point liquid, lower sediment thing and carry out homogeneous using high pressure microjet mode first, and taipei fritillary bulb ultrasonic cleaning and dispersion is used in supernatant circulating and recovering to step 1；
Step 4, the taipei fritillary bulb homogeneous solution obtained to step 3 by cold sterilization mode carries out ultra-high pressure sterilization, make sample that physical chemistry and the biological effects such as enzyme inactivation, protein denaturation, starch gelatinization and bacteria inactivation rate are produced under high pressure as pressure matchmaker using water, so as to reach sterilizing and modified purpose；
Step 5, taipei fritillary bulb homogeneous solution after being sterilized in step 4 is dried, drying uses spray drying, 70 DEG C of drying temperature, drying time 4h, dried taipei fritillary bulb obtains taipei fritillary bulb ultra micro freeze-dried powder product after crossing 800 mesh mesh screens, its moisture content is less than 3%, and average grain diameter is below 5 μm.
The above is preferred exemplary applications of the invention, not limitation of the present invention, and every simple modification made according to technical key point, structure change change are belonged within protection scope of the present invention.
Claims (7)
1. a kind of preparation method of taipei fritillary bulb ultra micro freeze-dried powder, it is characterised in that comprise the following steps：
Step 1, takes and dries standby taipei fritillary bulb sample, and being put into supersonic wave cleaning machine carries out cleaning and preliminary dispersion is crushed；
Step 2, the ultrasonically treated gained mixed liquor of step 1 is filtered, and filter cake and filter residue are used for mechanical jordaning, and filtrate carries out mechanical jordaning, taipei fritillary bulb slurries are obtained after mechanical jordaning with filter cake filter residue in the lump after sand core funnel filters off moisture to residual volume；
Step 3, the taipei fritillary bulb slurries to being obtained in step 2 carry out centrifugation point liquid, lower sediment thing and carry out homogeneous using high pressure microjet mode first, and supernatant is used for taipei fritillary bulb ultrasonic cleaning and dispersion in being recycled to step 1；
Step 4, the taipei fritillary bulb homogeneous solution obtained to step 3 by cold sterilization mode carries out ultra-high pressure sterilization, make sample that physical chemistry and the biological effects such as enzyme inactivation, protein denaturation, starch gelatinization and bacteria inactivation rate are produced under high pressure as pressure matchmaker using water, so as to reach sterilizing and modified purpose；
Step 5, taipei fritillary bulb ultra micro freeze-dried powder is obtained after being dried the taipei fritillary bulb homogeneous solution after being sterilized in step 4, cross sieve classification.
2. the preparation method of a kind of taipei fritillary bulb ultra micro freeze-dried powder according to claim 1, it is characterised in that the step 1 ultrasonication power is 200~600W, and 20 ~ 60min of batch process under room temperature condition, ultrasonication concentration is 30% ~ 60%.
3. the preparation method of a kind of taipei fritillary bulb ultra micro freeze-dried powder according to claim 1, it is characterised in that the step 2 carries out mechanical jordaning using PFI fiberizers, defibrination revolution is 1500r/min, grinding clearance 0.2mm, defibrination time 10min, 25 ± 5 DEG C of defibrination temperature.
4. the preparation method of a kind of taipei fritillary bulb ultra micro freeze-dried powder according to claim 1, it is characterised in that the drying of taipei fritillary bulb powder uses -50 DEG C of vacuum freeze dryings in the step 5, and drying time is 24h.
5. the preparation method of a kind of taipei fritillary bulb ultra micro freeze-dried powder according to claim 1, it is characterised in that the drying of taipei fritillary bulb powder uses spray drying, 60 ~ 80 DEG C of drying temperature, 4 ~ 5h of drying time in the step 5.
6. the preparation method of a kind of taipei fritillary bulb ultra micro freeze-dried powder according to claim 1, it is characterised in that dried taipei fritillary bulb powder obtains taipei fritillary bulb ultra micro freeze-dried powder after crossing the mesh screen of 800 mesh in the step 5.
7. the preparation method of a kind of taipei fritillary bulb ultra micro freeze-dried powder according to claim 1, it is characterised in that the moisture content of taipei fritillary bulb ultra micro freeze-dried powder prepared by methods described is less than 3%, and average grain diameter is below 5 μm.
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| CN201510942235.7A CN106880737A (en) | 2015-12-16 | 2015-12-16 | A kind of preparation method of taipei fritillary bulb ultra micro freeze-dried powder |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109090457A (en) * | 2018-08-27 | 2018-12-28 | 怀宁县荣升食品厂 | A kind of bulbus fritillariae cirrhosae cake and preparation method thereof |
| CN114832061A (en) * | 2022-05-30 | 2022-08-02 | 重庆市中药研究院 | Processing method of fritillaria taipaiensis |
-
2015
- 2015-12-16 CN CN201510942235.7A patent/CN106880737A/en not_active Withdrawn
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109090457A (en) * | 2018-08-27 | 2018-12-28 | 怀宁县荣升食品厂 | A kind of bulbus fritillariae cirrhosae cake and preparation method thereof |
| CN114832061A (en) * | 2022-05-30 | 2022-08-02 | 重庆市中药研究院 | Processing method of fritillaria taipaiensis |
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Application publication date: 20170623 |