CN106052304A - Radix tetrastigme drying method - Google Patents
Radix tetrastigme drying method Download PDFInfo
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- CN106052304A CN106052304A CN201610592284.7A CN201610592284A CN106052304A CN 106052304 A CN106052304 A CN 106052304A CN 201610592284 A CN201610592284 A CN 201610592284A CN 106052304 A CN106052304 A CN 106052304A
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- radix
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- apioris fortunei
- lespedezae buergeri
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- 239000010409 thin film Substances 0.000 claims abstract description 22
- 239000002994 raw material Substances 0.000 claims abstract description 8
- 238000001816 cooling Methods 0.000 claims description 27
- 238000010792 warming Methods 0.000 claims description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 10
- 239000003814 drug Substances 0.000 claims description 5
- 238000004140 cleaning Methods 0.000 claims description 3
- 238000004321 preservation Methods 0.000 claims description 3
- 238000007710 freezing Methods 0.000 abstract description 16
- 230000008014 freezing Effects 0.000 abstract description 16
- 238000000034 method Methods 0.000 abstract description 13
- 230000000694 effects Effects 0.000 abstract description 9
- 230000000717 retained effect Effects 0.000 abstract description 3
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- 238000004108 freeze drying Methods 0.000 description 6
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- 241000219094 Vitaceae Species 0.000 description 1
- 235000009754 Vitis X bourquina Nutrition 0.000 description 1
- 235000012333 Vitis X labruscana Nutrition 0.000 description 1
- 240000006365 Vitis vinifera Species 0.000 description 1
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- 208000026435 phlegm Diseases 0.000 description 1
- 231100000614 poison Toxicity 0.000 description 1
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Classifications
-
- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F26—DRYING
- F26B—DRYING SOLID MATERIALS OR OBJECTS BY REMOVING LIQUID THEREFROM
- F26B1/00—Preliminary treatment of solid materials or objects to facilitate drying, e.g. mixing or backmixing the materials to be dried with predominantly dry solids
-
- 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)
- A61K36/185—Magnoliopsida (dicotyledons)
- A61K36/48—Fabaceae or Leguminosae (Pea or Legume family); Caesalpiniaceae; Mimosaceae; Papilionaceae
-
- 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)
- A61K36/185—Magnoliopsida (dicotyledons)
- A61K36/87—Vitaceae or Ampelidaceae (Vine or Grape family), e.g. wine grapes, muscadine or peppervine
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61P—SPECIFIC THERAPEUTIC ACTIVITY OF CHEMICAL COMPOUNDS OR MEDICINAL PREPARATIONS
- A61P11/00—Drugs for disorders of the respiratory system
- A61P11/04—Drugs for disorders of the respiratory system for throat disorders
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61P—SPECIFIC THERAPEUTIC ACTIVITY OF CHEMICAL COMPOUNDS OR MEDICINAL PREPARATIONS
- A61P17/00—Drugs for dermatological disorders
- A61P17/02—Drugs for dermatological disorders for treating wounds, ulcers, burns, scars, keloids, or the like
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61P—SPECIFIC THERAPEUTIC ACTIVITY OF CHEMICAL COMPOUNDS OR MEDICINAL PREPARATIONS
- A61P19/00—Drugs for skeletal disorders
- A61P19/04—Drugs for skeletal disorders for non-specific disorders of the connective tissue
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61P—SPECIFIC THERAPEUTIC ACTIVITY OF CHEMICAL COMPOUNDS OR MEDICINAL PREPARATIONS
- A61P19/00—Drugs for skeletal disorders
- A61P19/08—Drugs for skeletal disorders for bone diseases, e.g. rachitism, Paget's disease
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61P—SPECIFIC THERAPEUTIC ACTIVITY OF CHEMICAL COMPOUNDS OR MEDICINAL PREPARATIONS
- A61P29/00—Non-central analgesic, antipyretic or antiinflammatory agents, e.g. antirheumatic agents; Non-steroidal antiinflammatory drugs [NSAID]
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61P—SPECIFIC THERAPEUTIC ACTIVITY OF CHEMICAL COMPOUNDS OR MEDICINAL PREPARATIONS
- A61P31/00—Antiinfectives, i.e. antibiotics, antiseptics, chemotherapeutics
- A61P31/04—Antibacterial agents
- A61P31/06—Antibacterial agents for tuberculosis
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61P—SPECIFIC THERAPEUTIC ACTIVITY OF CHEMICAL COMPOUNDS OR MEDICINAL PREPARATIONS
- A61P39/00—General protective or antinoxious agents
- A61P39/02—Antidotes
-
- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F26—DRYING
- F26B—DRYING SOLID MATERIALS OR OBJECTS BY REMOVING LIQUID THEREFROM
- F26B1/00—Preliminary treatment of solid materials or objects to facilitate drying, e.g. mixing or backmixing the materials to be dried with predominantly dry solids
- F26B1/005—Preliminary treatment of solid materials or objects to facilitate drying, e.g. mixing or backmixing the materials to be dried with predominantly dry solids by means of disintegrating, e.g. crushing, shredding, milling the materials to be dried
-
- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F26—DRYING
- F26B—DRYING SOLID MATERIALS OR OBJECTS BY REMOVING LIQUID THEREFROM
- F26B7/00—Drying solid materials or objects by processes using a combination of processes not covered by a single one of groups F26B3/00 and F26B5/00
-
- 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
- A61K2236/17—Preparation or pretreatment of starting material involving drying, e.g. sun-drying or wilting
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- Health & Medical Sciences (AREA)
- Engineering & Computer Science (AREA)
- Life Sciences & Earth Sciences (AREA)
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- Pharmacology & Pharmacy (AREA)
- General Health & Medical Sciences (AREA)
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- Chemical Kinetics & Catalysis (AREA)
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- Oncology (AREA)
- Toxicology (AREA)
- Medicines Containing Plant Substances (AREA)
- Medicinal Preparation (AREA)
- Drying Of Solid Materials (AREA)
Abstract
The invention relates to a radix tetrastigme drying method which comprises the steps of radix tetrastigme raw material slicing, thin film laying for freezing, drying at the first stage and drying at the second stage. According to the radix tetrastigme drying method, by reasonable setting of parameters such as the time of thin film laying for freezing and the drying durations at the first and second stages as well as the temperature and the pressure, the activity of radix tetrastigme can be retained more completely after the radix tetrastigme is dried; effective components of the radix tetrastigme dried by the method disclosed by the invention can be retained to the maximum extent; furthermore, a finished product is high in breakage resistance performance; the dried radix tetrastigme finished product can be prepared into electuary, an oral preparation and the like.
Description
Technical field
The present invention relates to Radix Apioris Fortunei (Radix Lespedezae Buergeri) drying means.
Background technology
Radix Apioris Fortunei (Radix Lespedezae Buergeri), rectification of name: tetratigma hemsleyanum, have another name called gold thread hoist, Radix Tetrastigmatis Hemsleyani, stone mouse, belong to Rhamnales, Vitaceae grass
Matter liana.Herb all can be used as medicine, and the medicinal effects with underground tuber and fruit is best.The agents area of Chinese crude drug Radix Apioris Fortunei (Radix Lespedezae Buergeri) is Portugal
Tuber, fruit or the herb of grape section Tetrastigma plant Radix Apioris Fortunei (Radix Lespedezae Buergeri), can gather, dry or using fresh herb the whole year.Its property is flat,
Mildly bitter flavor, has the effects such as heat-clearing and toxic substances removing, dispelling pathogenic wind and eliminating phlegm, promoting blood circulation and stopping pain, cure mainly venom, tonsillitis, tuberculous lymphadenitis,
The disease such as traumatic injury, children with high fever induced convulsions.
Traditional Radix Apioris Fortunei (Radix Lespedezae Buergeri) drying and processing method, dries section and packs after stifling.During drying, Radix Apioris Fortunei (Radix Lespedezae Buergeri)
Essence substance run off serious, the most destroyed, reduce its drug effect, and its water content be high, the most mouldy and rotten, be difficult to storage
Deposit.
Other existing Radix Apioris Fortunei (Radix Lespedezae Buergeri) drying meanss, such as vacuum drying, are usually present energy consumption higher, and Product Activity loss is big,
The shortcomings such as finished product loosens frangible, and transport storage is inconvenient.
Summary of the invention
The present invention relates to Radix Apioris Fortunei (Radix Lespedezae Buergeri) drying means, for existing issue, it is possible to make the dried finished activated guarantor of Radix Apioris Fortunei (Radix Lespedezae Buergeri)
Stay more complete, and do not loosen.
The present invention is achieved by the following technical solutions:
Radix Apioris Fortunei (Radix Lespedezae Buergeri) drying means, in turn includes the following steps:
A, by Radix Apioris Fortunei (Radix Lespedezae Buergeri) feed stock chip, for making follow-up dry Radix Apioris Fortunei (Radix Lespedezae Buergeri) the most thorough uniformly, thickness is preferably 2mm ~ 5mm.
B, will section after Radix Apioris Fortunei (Radix Lespedezae Buergeri) be layered on thin film, be cooled to-13 DEG C ~-19.5 DEG C, cooling rate is 33 DEG C per hour
~ 39.5 DEG C, then keep temperature 2.5 ~ 3 hours；Sublimation drying could be carried out under vacuo, otherwise after only product all freezes
In the presence of having partially liq, the most not only can evaporate rapidly, cause the concentration of liquid to make the volume-diminished of freeze-drying prods；And
And the gas being dissolved in water can come up rapidly under vacuo, cause the appearance as liquid boiling, make freeze-drying prods bubbling.
Film pad is below, thin film holds Radix Apioris Fortunei (Radix Lespedezae Buergeri), its benefit is so that Radix Apioris Fortunei (Radix Lespedezae Buergeri) lowering temperature uniform, uniform drying,
Can reduce the waste of the energy, be lost little, recovery rate is high；Reduce the probability of cross-contamination, it is ensured that the hygiology of Radix Apioris Fortunei (Radix Lespedezae Buergeri)
Qualified rate is high；Decrease the cleaning of freeze dryer simultaneously；Overlay film maintains to pass for improving Radix Apioris Fortunei (Radix Lespedezae Buergeri) quality and drug effect
Important effect.Cooling rate is 33 DEG C per hour ~ 39.5 DEG C, and for the most freezing, the most freezing ice crystal produced is relatively big, is dried
Speed is very fast, and the lyophilizing for Radix Apioris Fortunei (Radix Lespedezae Buergeri) is helpful, and temperature controls at-13 DEG C ~-19.5 DEG C, and one ensure that freezing temperature
Spending of a sufficiently low, two eutectic points being because Radix Apioris Fortunei (Radix Lespedezae Buergeri) material are about-8 DEG C ~-5 DEG C, and cryogenic temperature is being taken the photograph less than eutectic point 5 to 10
When family name spends, the activity of Radix Apioris Fortunei (Radix Lespedezae Buergeri) retains more abundant, and cryogenic temperature be gradually lowered the control with the time, make Radix Apioris Fortunei (Radix Lespedezae Buergeri) freeze more
Uniformly, more solid, more thoroughly, be conducive to the distillation of moisture below, the water content making final finished is lower, improves stablizing of product
Property.
C, the system absolute pressure of being evacuated to are 75 ~ 100Pa, are warming up to 45 ~ 50 DEG C, programming rate is 1.9 DEG C per hour ~
2.3 DEG C, keep absolute pressure and temperature 25 ~ 30 hours；During cooling, the temperature starting to separate out crystal claims the freezing point of solution, and molten
The temperature that liquid all condenses is freezing point.Because freezing point is exactly the starting point (fusing point) of fusing, for solution, then it is molten
Matter and the common melting point of menstruum, be eutectic point.The sublimation drying stage to ensure that the temperature at distillation interface is less than temperature of eutectic point,
And make sublimation temperature close to its eutectic point but have to be lower than eutectic point as far as possible, and if the temperature of distillation is too low, then the effect distilled
Rate reduces, and the temperature of distillation is if above temperature of eutectic point, then product can melt, and the concentration of solution can make lyophilizing produce under vacuo
The volume-diminished of product, the gas in solution can come up rapidly under vacuo and make freeze-drying prods bubbling, be unfavorable for that Radix Apioris Fortunei (Radix Lespedezae Buergeri) is dried
Stable and the reservation of drug effect of finished product.And the system absolute pressure of selection is 75 ~ 100Pa, temperature controls, at 45 ~ 50 DEG C, to be because
In material, moisture molten some boiling point under negative pressure state all reduces along with the raising of vacuum, this absolute pressure and the setting of temperature
It is optimum selection, and drying time is 25 ~ 30 hours, it is ensured that being fully dried of Radix Apioris Fortunei (Radix Lespedezae Buergeri), lay the foundation for subsequent step.
D, system absolute pressure being risen to 25 ~ 40Pa, temperature is down to 18 ~ 30 DEG C, and cooling rate is per hour 15 DEG C ~ 32
DEG C, keep absolute pressure and temperature 1-2.5 hour.After this step, the water content of Radix Apioris Fortunei (Radix Lespedezae Buergeri) is less than 2%.After step C,
Eliminate the moisture of about 90%, also retention and have the moisture distribution of about 10% on the capillary wall and polarity gene of Radix Apioris Fortunei (Radix Lespedezae Buergeri), these
The existence of moisture, can cause some chemical reactions, causes bacteria breed, thus affects the blue and green quality being dried to product of SANYE and steady
Fixed.And the reason still possessing absolute pressure 25 ~ 40Pa is, under vacuum condition, it is ensured that the Radix Apioris Fortunei (Radix Lespedezae Buergeri) not the most thoroughly being dried is not
By air pollution, temperature reduces to 18 ~ 30 DEG C, on the one hand, this temperature range, reasonably controls heat input, can prevent from producing
Product overdrying, on the other hand, this temperature range is normal temperature condition, can effectively save the energy, prevent the waste of the energy.
As the improvement further of the present invention, the thin film in step B is arranged alternately above with Radix Apioris Fortunei (Radix Lespedezae Buergeri).First in lyophilizing
The pallet upper berth ground floor thin film of machine, then blue or green at ground floor thin film upper berth Top-three Leaves, then on this layer of Radix Apioris Fortunei (Radix Lespedezae Buergeri), cover the
Two-layer film, then at second layer thin film upper berth Radix Apioris Fortunei (Radix Lespedezae Buergeri), thin film is arranged alternately above successively with Radix Apioris Fortunei (Radix Lespedezae Buergeri), on the one hand improves sky
Between utilization rate, on the other hand Radix Apioris Fortunei (Radix Lespedezae Buergeri) can be made to be dried lowering temperature uniform, be also prevented from polluting.
As the improvement further of the present invention, thin film is selected has hydrophobicity, does not gets wet, dust-proof, and can allow steam
The thin film passed through, thickness is 90 ~ 100um.Film material is selected containing politef, and the thin film of this material and specification has
Hydrophobicity, does not gets wet, dust-proof, anti-powder, but can allow the characteristic that steam passes through, it is ensured that it is thorough that Radix Apioris Fortunei (Radix Lespedezae Buergeri) is dried.
As the improvement further of the present invention, before step A, also include cleaning raw material, drain raw material.By Radix Apioris Fortunei (Radix Lespedezae Buergeri)
Raw material is carried out, and drains process, can improve the sanitary index of Radix Apioris Fortunei (Radix Lespedezae Buergeri).
As the improvement further of the present invention, the Radix Apioris Fortunei (Radix Lespedezae Buergeri) after step D is crushed to 60 mesh, then carries out physics and break
Wall, then seal preservation, make medicament.Radix Apioris Fortunei (Radix Lespedezae Buergeri) under coarse powder state carries out physical wall breaking, and physical wall breaking is at hermetically drying bar
Under part, with two strands of supersonic airstreams, SANYE Calomelas is clashed into.
As the improvement further of the present invention, in step B, being cooled to-18 DEG C, cooling rate is 38 DEG C per hour, so
Rear holding temperature 2.5 hours.This Parameter Conditions, for a kind of selection of Radix Apioris Fortunei (Radix Lespedezae Buergeri) freezing parameter.
As the improvement further of the present invention, in step B, being cooled to-14 DEG C, cooling rate is 34 DEG C per hour, so
Rear holding temperature 2.8 hours.This Parameter Conditions, for the another kind of selection of Radix Apioris Fortunei (Radix Lespedezae Buergeri) freezing parameter.
As the improvement further of the present invention, in step C, system absolute pressure is 80Pa, and temperature is 48 DEG C, keeps absolutely
To pressure and temperature 28 hours.This Parameter Conditions, for a kind of selection of Radix Apioris Fortunei (Radix Lespedezae Buergeri) first stage drying parameter.
As the improvement further of the present invention, in step C, system absolute pressure is 90Pa, and temperature is 46 DEG C, keeps absolutely
To pressure and temperature 26 hours.This Parameter Conditions, for the another kind of selection of Radix Apioris Fortunei (Radix Lespedezae Buergeri) first stage drying parameter.
As the improvement further of the present invention, in step D, system absolute pressure is 30Pa, and temperature is 25 DEG C, keeps absolutely
To pressure and temperature 1.5 hours.This Parameter Conditions, for a kind of selection of Radix Apioris Fortunei (Radix Lespedezae Buergeri) second stage drying parameter.
According to Radix Apioris Fortunei (Radix Lespedezae Buergeri) drying means of the present invention, the Radix Apioris Fortunei (Radix Lespedezae Buergeri) active component content of preparation is high, and product is non-friable, it is simple to storage
Deposit and transport.Main cause has:
(1), use thin film to underlay, thin film repave one layer of Radix Apioris Fortunei (Radix Lespedezae Buergeri), the method that thin film and Radix Apioris Fortunei (Radix Lespedezae Buergeri) are alternately superimposed on so that
The content of final Radix Apioris Fortunei (Radix Lespedezae Buergeri) active component total flavones is higher, and reason is that thin film makes Radix Apioris Fortunei (Radix Lespedezae Buergeri) lowering temperature uniform, also prevent SANYE
Green grass or young crops is secondary polluted, it is ensured that the Hygienic Index qualification rate of Radix Apioris Fortunei (Radix Lespedezae Buergeri) is high, effective ingredient purity higher, more filling of reservation
Point.
(2), the drying means of the present invention freezing stage in stepb makes raw material be in-13 DEG C ~-19.5 DEG C states, freezing temperature
Spending less than eutectic point 5 to 10 degrees Celsius, the activity of Radix Apioris Fortunei (Radix Lespedezae Buergeri) retains more abundant, decreases the loss of Flavonoid substances.
It is an advantage of the invention that while being effectively retained Radix Apioris Fortunei (Radix Lespedezae Buergeri) active component, processing technique is simple, and end product quality is higher,
Not easily broken.
Accompanying drawing explanation
The parametric plot of the Radix Apioris Fortunei (Radix Lespedezae Buergeri) drying means that Fig. 1 provides for the embodiment of the present invention 1.
The parametric plot of the Radix Apioris Fortunei (Radix Lespedezae Buergeri) drying means that Fig. 2 provides for the embodiment of the present invention 2.
The parametric plot of the Radix Apioris Fortunei (Radix Lespedezae Buergeri) drying means that Fig. 3 provides for the embodiment of the present invention 3.
The parametric plot of the Radix Apioris Fortunei (Radix Lespedezae Buergeri) drying means that Fig. 4 provides for the embodiment of the present invention 4.
The parametric plot of the Radix Apioris Fortunei (Radix Lespedezae Buergeri) drying means that Fig. 5 provides for the embodiment of the present invention 5.
The parametric plot of the Radix Apioris Fortunei (Radix Lespedezae Buergeri) drying means that Fig. 6 provides for the embodiment of the present invention 6.
The parametric plot of the Radix Apioris Fortunei (Radix Lespedezae Buergeri) drying means that Fig. 7 provides for the embodiment of the present invention 7.
Detailed description of the invention
By further illustrating the technological means and effect that the present invention taked by realizing predetermined goal of the invention, below fasten
Accompanying drawing and preferred embodiment, to the foundation detailed description of the invention of the present invention, structure, feature and effect thereof, after describing in detail such as.Real
Execute the freeze dryer in example and all use LYO-30m2Type vacuum freeze drier.
Radix Apioris Fortunei (Radix Lespedezae Buergeri) effective ingredient contains total flavones, the mensuration to general flavone content, uses UV-VIS spectrophotometry, with reed
Fourth is reference substance, at wavelength 500nm, the total flavones in Radix Apioris Fortunei (Radix Lespedezae Buergeri) is carried out assay.
And the chip resistant ability of Radix Apioris Fortunei (Radix Lespedezae Buergeri), then use coherent detection instrument, balance and blower fan inspection.Adjusting instrument rotating speed is 25
Rpm, experimental period is 4 minutes, the rotary drum of instrument 100 times.Take trial target 10 every time, blow away its table with blower fan
The powder in face, weighs.Trial target through measuring being put in the cylinder of instrument, starts motor rotation cylinder 100 times, rotation terminates
After, checkout facility product shatter number, then blow away powder with blower fan, weigh, with the weight that the difference of the amount of taking is less loss.
The water content of Radix Apioris Fortunei (Radix Lespedezae Buergeri) finished product, uses infrared ray fast tester for water content to measure.
Embodiment 1
Radix Apioris Fortunei (Radix Lespedezae Buergeri) drying means, step is:
A, by Radix Apioris Fortunei (Radix Lespedezae Buergeri) feed stock chip, thickness is 2mm；
B, will section after Radix Apioris Fortunei (Radix Lespedezae Buergeri) be layered on the polytetrafluoroethylene film that thickness is 90um, be cooled to-13 DEG C ~ DEG C, cooling speed
Degree is 33 DEG C per hour, then keeps temperature 3 hours；
C, the system absolute pressure of being evacuated to are 75Pa, are warming up to 50 DEG C, and programming rate is 1.9 DEG C per hour, keep absolute pressure
Power and temperature 30 hours；
D, system absolute pressure being risen to 25Pa, temperature is down to 30 DEG C, and cooling rate is 20 DEG C per hour, keep absolute pressure and
Temperature 2.5 hours.Design parameter change refers to Fig. 1.
Embodiment 2
Radix Apioris Fortunei (Radix Lespedezae Buergeri) drying means, step is:
A, by Radix Apioris Fortunei (Radix Lespedezae Buergeri) feed stock chip, thickness is 3mm；
B, will section after Radix Apioris Fortunei (Radix Lespedezae Buergeri) be layered on the polytetrafluoroethylene film that thickness is 100um, be cooled to-14 DEG C, cooling rate
For per hour 34 DEG C, then keep temperature 2.9 hours；
C, the system absolute pressure of being evacuated to are 80Pa, are warming up to 49 DEG C, and programming rate is 2.1 DEG C per hour, keep absolute pressure
Power and temperature 29 hours；
D, system absolute pressure being risen to 30Pa, temperature is down to 25 DEG C, and cooling rate is 24 DEG C per hour, keep absolute pressure and
Temperature 2 hours.Design parameter change refers to Fig. 2.
Embodiment 3
Radix Apioris Fortunei (Radix Lespedezae Buergeri) drying means, step is:
A, by Radix Apioris Fortunei (Radix Lespedezae Buergeri) feed stock chip, thickness is 4mm；
B, will section after Radix Apioris Fortunei (Radix Lespedezae Buergeri) be layered on the polytetrafluoroethylene film that thickness is 100um, be cooled to-16 DEG C, cooling rate
For per hour 36 DEG C, then keep temperature 2.7 hours；
C, the system absolute pressure of being evacuated to are 85Pa, are warming up to 48 DEG C, and programming rate is 2.1 DEG C per hour, keep absolute pressure
Power and temperature 28 hours；
D, system absolute pressure being risen to 35Pa, temperature is down to 20 DEG C, and cooling rate is 28 DEG C per hour, keep absolute pressure and
Temperature 1.5 hours.Design parameter change refers to Fig. 3.
Embodiment 4
Radix Apioris Fortunei (Radix Lespedezae Buergeri) drying means, step is:
A, by Radix Apioris Fortunei (Radix Lespedezae Buergeri) feed stock chip, thickness is 5mm；
B, will section after Radix Apioris Fortunei (Radix Lespedezae Buergeri) be layered on the polytetrafluoroethylene film that thickness is 100um, be cooled to-18 DEG C, cooling rate
For per hour 38 DEG C, then keep temperature 2.6 hours；
C, the system absolute pressure of being evacuated to are 95Pa, are warming up to 47 DEG C, and programming rate is 2.2 DEG C per hour, keep absolute pressure
Power and temperature 27 hours；
D, system absolute pressure being risen to 40Pa, temperature is down to 19 DEG C, and cooling rate is 30 DEG C per hour, keep absolute pressure and
Temperature 1.2 hours.Design parameter change refers to Fig. 4.
Embodiment 5
Radix Apioris Fortunei (Radix Lespedezae Buergeri) drying means, step is:
A, by Radix Apioris Fortunei (Radix Lespedezae Buergeri) feed stock chip, thickness is 3mm；
B, will section after Radix Apioris Fortunei (Radix Lespedezae Buergeri) be layered on the polytetrafluoroethylene film that thickness is 100um, be cooled to-19.5 DEG C, cooling speed
Degree is 39.5 DEG C per hour, then keeps temperature 2.5 hours；
C, the system absolute pressure of being evacuated to are 100Pa, are warming up to 45 DEG C, and programming rate is 2.3 DEG C per hour, keep absolute pressure
Power and temperature 25 hours；
D, system absolute pressure being risen to 40Pa, temperature is down to 18 DEG C, and cooling rate is 32 DEG C per hour, keep absolute pressure and
Temperature 1 hour.Design parameter change refers to Fig. 5.
Embodiment 6
Radix Apioris Fortunei (Radix Lespedezae Buergeri) drying means, step is:
A, by Radix Apioris Fortunei (Radix Lespedezae Buergeri) feed stock chip, thickness is 3mm；
B, will section after Radix Apioris Fortunei (Radix Lespedezae Buergeri) be layered on the polytetrafluoroethylene film that thickness is 100um, be cooled to-18 DEG C, cooling rate
For per hour 38 DEG C, then keep temperature 2.5 hours；
C, the system absolute pressure of being evacuated to are 80Pa, are warming up to 48 DEG C, and programming rate is 2.0 DEG C per hour, keep absolute pressure
Power and temperature 28 hours；
D, system absolute pressure being risen to 30Pa, temperature is down to 25 DEG C, and cooling rate is 23 DEG C per hour, keep absolute pressure and
Temperature 1.5 hours.Design parameter change refers to Fig. 6.
Embodiment 7
Radix Apioris Fortunei (Radix Lespedezae Buergeri) drying means, step is:
A, by Radix Apioris Fortunei (Radix Lespedezae Buergeri) feed stock chip, thickness is 3mm；
B, will section after Radix Apioris Fortunei (Radix Lespedezae Buergeri) be layered on the polytetrafluoroethylene film that thickness is 100um, be cooled to-14 DEG C, cooling rate
For per hour 34 DEG C, then keep temperature 2.8 hours；
C, the system absolute pressure of being evacuated to are 90Pa, are warming up to 46 DEG C, and programming rate is 2.1 DEG C per hour, keep absolute pressure
Power and temperature 26 hours；
D, system absolute pressure being risen to 30Pa, temperature is down to 25 DEG C, and cooling rate is 20 DEG C per hour, keep absolute pressure and
Temperature 1.2 hours.Design parameter change refers to Fig. 7.
Embodiment 8
On the basis of embodiment 6, before step A, Radix Apioris Fortunei (Radix Lespedezae Buergeri) raw material is carried out, drains；After step D, by three
Leaf Calomelas is broken to 60 mesh, then carries out physical wall breaking, then seals preservation, makes medicament.Other steps and parameter constant.
Measure the water content of each embodiment Radix Apioris Fortunei (Radix Lespedezae Buergeri) finished product, and the Radix Apioris Fortunei (Radix Lespedezae Buergeri) detecting above-mentioned eight embodiments is dried finished product
General flavone content, chip resistant ability, result is as follows:
| Embodiment | 1 | 2 | 3 | 4 | 5 | 6 | 7 | 8 |
| Total flavones (mg/g) | 7.55 | 7.45 | 7.55 | 7.50 | 7.53 | 7.65 | 7.60 | 7.64 |
| Shatter (individual) | Nothing | Nothing | 1 | 1 | 1 | Nothing | Nothing | Nothing |
| Water content (%) | 1.7 | 1.8 | 1.9 | 1.6 | 1.7 | 1.6 | 1.7 | 1.9 |
According to above-described embodiment result, the general flavone content of final dried Radix Apioris Fortunei (Radix Lespedezae Buergeri) is in the scope of 7.45-7.65mg/g, anti-
Fragmentation ability is preferable, and water content is less than 2%, drying means of the present invention so that the indices of Radix Apioris Fortunei (Radix Lespedezae Buergeri) all reaches
Excellent state.Below by Experimental Comparison example, usefulness of the present invention being described, Experimental Comparison example is intended to further illustrate the present invention
Usefulness, rather than limitation of the present invention.
Comparative example
Taking and be processed as follows with a collection of fresh Radix Apioris Fortunei (Radix Lespedezae Buergeri), the described Radix Apioris Fortunei (Radix Lespedezae Buergeri) that fresh Radix Apioris Fortunei (Radix Lespedezae Buergeri) is in this specification is former
Material.
(1) drying Radix Apioris Fortunei (Radix Lespedezae Buergeri): fresh Radix Apioris Fortunei (Radix Lespedezae Buergeri), cut into slices 5mm, 60 DEG C of drying.
(2) vacuum drying: fresh Radix Apioris Fortunei (Radix Lespedezae Buergeri), cut into slices 5mm, baking temperature 60 DEG C, vacuum 0.09MPa.
(3) drying means of the present invention: fresh Radix Apioris Fortunei (Radix Lespedezae Buergeri), cut into slices 5mm, and paving thin film is freezing, and the Radix Apioris Fortunei (Radix Lespedezae Buergeri) after will cutting into slices is layered on
On thin film, being cooled to-18 DEG C, cooling rate is 38 DEG C per hour, then keeps temperature 2.5 hours；First drying stage, takes out true
Empty is 80Pa to system absolute pressure, is warming up to 48 DEG C, and programming rate is 2 DEG C per hour, keeps absolute pressure and temperature 28 little
Time；Second drying stage, rises to 30Pa by system absolute pressure, and temperature is down to 25 DEG C, and cooling rate is 20 DEG C per hour, keeps
Absolute pressure and temperature 1.5 hours.
(4) other freeze drying process one: fresh Radix Apioris Fortunei (Radix Lespedezae Buergeri), cut into slices 5mm, and sabot is freezing, and the Radix Apioris Fortunei (Radix Lespedezae Buergeri) after will cutting into slices directly is put
Putting on pallet, be cooled to-18 DEG C, cooling rate is 38 DEG C per hour, then keeps temperature 2.5 hours；First drying stage,
The system absolute pressure of being evacuated to is 80Pa, is warming up to 48 DEG C, and programming rate is 2 DEG C per hour, keeps absolute pressure and temperature
28 hours；Second drying stage, rises to 30Pa by system absolute pressure, and temperature is down to 25 DEG C, and cooling rate is 20 DEG C per hour,
Keep absolute pressure and temperature 1.5 hours.
(5) other freeze drying process two: fresh Radix Apioris Fortunei (Radix Lespedezae Buergeri), shave, sabot is freezing, gradually after cooling 3 hours to-20 DEG C cold
Freezing, it is 60Pa that sublimation stage is evacuated to system absolute pressure, is warming up to 40 DEG C, sublimation drying 15 ~ 24 hours, resolution phase temperature
Degree controls at 35 ~ 65 DEG C, 7 hours retention times, discharging.
(6) fresh Radix Apioris Fortunei (Radix Lespedezae Buergeri), without any process.
The effective ingredient general flavone content of Radix Apioris Fortunei (Radix Lespedezae Buergeri) obtained by above-mentioned several method is dried and to Radix Apioris Fortunei (Radix Lespedezae Buergeri) chip resistant energy
Power detects, and result is as follows:
| Drying means | (1) dry | (2) vacuum drying | (3) present invention | (4) additive method one | (5) additive method two | (6) fresh goods |
| Total flavones (mg/g) | 6.33±0.11 | 6.61±0.15 | 7.55±0.10 | 7.21±0.10 | 7.10±0.11 | 7.65±0.20 |
| Shatter (individual) | Nothing | Nothing | 1 | 3 | 5 | Nothing |
| Loss amount (%) | 0.65 | 0.66 | 1.25 | 2.86 | 6.21 | Nothing |
It can be seen from the results above that use forwarding method of the present invention be dried obtained by Radix Apioris Fortunei (Radix Lespedezae Buergeri) total flavones amount compared to other four kinds
Method be dried obtained by the total flavones amount of Radix Apioris Fortunei (Radix Lespedezae Buergeri) higher, other two kinds of freeze drying process of chip resistant energy force rate are preferable.
The above, be only presently preferred embodiments of the present invention, and the present invention not makees any pro forma restriction, though
So the present invention discloses as above with preferred embodiment, but is not limited to the present invention, and any those skilled in the art, not
In the range of departing from technical solution of the present invention, when the technology contents of available the disclosure above makes a little change or is modified to equivalent change
The Equivalent embodiments changed, as long as being without departing from technical solution of the present invention content, implements above according to the technical spirit of the present invention
Any simple modification, equivalent variations and the modification that example is made, all still falls within the range of technical solution of the present invention.
Claims (10)
1. Radix Apioris Fortunei (Radix Lespedezae Buergeri) drying means, it is characterised in that in turn include the following steps:
A, by Radix Apioris Fortunei (Radix Lespedezae Buergeri) feed stock chip, thickness is 2mm ~ 5mm；
B, the Radix Apioris Fortunei (Radix Lespedezae Buergeri) after section being layered on thin film, be cooled to-13 DEG C ~-19.5 DEG C, cooling rate is 33 DEG C per hour ~
39.5 DEG C, then keep temperature 2.5 ~ 3 hours；
C, the system absolute pressure of being evacuated to are 75 ~ 100Pa, are warming up to 45 ~ 50 DEG C, and programming rate is per hour 1.9 DEG C ~ 2.3
DEG C, keep absolute pressure and temperature 25 ~ 30 hours；
D, system absolute pressure being risen to 25 ~ 40Pa, temperature is down to 18 ~ 30 DEG C, and cooling rate is 15 DEG C per hour ~ 32 DEG C, protects
Hold absolute pressure and temperature 1-2.5 hour.
2. Radix Apioris Fortunei (Radix Lespedezae Buergeri) drying means as claimed in claim 1, it is characterised in that the thin film in step B is with Radix Apioris Fortunei (Radix Lespedezae Buergeri) alternately
Stacked.
3. Radix Apioris Fortunei (Radix Lespedezae Buergeri) drying means as claimed in claim 2, it is characterised in that described thin film is selected has hydrophobicity, non-sticky
Water, dust-proof, and can allow the thin film that steam passes through, thickness is 90 ~ 100um.
4. the Radix Apioris Fortunei (Radix Lespedezae Buergeri) drying means as described in claim 1 or 2 or 3, it is characterised in that before step A, also includes cleaning
Raw material, drains raw material.
5. the Radix Apioris Fortunei (Radix Lespedezae Buergeri) drying means as described in claim 1 or 2 or 3, it is characterised in that the Radix Apioris Fortunei (Radix Lespedezae Buergeri) after step D is pulverized
To 60 mesh, then carry out physical wall breaking, then seal preservation, make medicament.
6. the Radix Apioris Fortunei (Radix Lespedezae Buergeri) drying means as described in claim 1 or 2 or 3, it is characterised in that in step B, be cooled to-18 DEG C, fall
Temperature speed is 38 DEG C per hour, then keeps temperature 2.5 hours.
7. the Radix Apioris Fortunei (Radix Lespedezae Buergeri) drying means as described in claim 1 or 2 or 3, it is characterised in that in step B, be cooled to-14 DEG C, fall
Temperature speed is 34 DEG C per hour, then keeps temperature 2.8 hours.
8. the Radix Apioris Fortunei (Radix Lespedezae Buergeri) drying means as described in claim 1 or 2 or 3, it is characterised in that in step C, system absolute pressure is
80Pa, temperature is 48 DEG C, keeps absolute pressure and temperature 28 hours.
9. the Radix Apioris Fortunei (Radix Lespedezae Buergeri) drying means as described in claim 1 or 2 or 3, it is characterised in that in step C, system absolute pressure is
90Pa, temperature is 46 DEG C, keeps absolute pressure and temperature 26 hours.
10. the Radix Apioris Fortunei (Radix Lespedezae Buergeri) drying means as described in claim 1 or 2 or 3, it is characterised in that in step D, system absolute pressure
For 30Pa, temperature is 25 DEG C, keeps absolute pressure and temperature 1.5 hours.
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| CN201811337486.2A CN109373704A (en) | 2016-07-26 | 2016-07-26 | Radix tetrastigme drying means |
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| CN115957870A (en) * | 2022-12-29 | 2023-04-14 | 武夷山元生泰生物科技有限公司 | Ultrafine grinding method for radix tetrastigme |
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