CN109248178A - A kind of filter method in Venenum Bufonis Injection preparation process - Google Patents
A kind of filter method in Venenum Bufonis Injection preparation process Download PDFInfo
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- CN109248178A CN109248178A CN201811222376.1A CN201811222376A CN109248178A CN 109248178 A CN109248178 A CN 109248178A CN 201811222376 A CN201811222376 A CN 201811222376A CN 109248178 A CN109248178 A CN 109248178A
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K35/00—Medicinal preparations containing materials or reaction products thereof with undetermined constitution
- A61K35/56—Materials from animals other than mammals
- A61K35/65—Amphibians, e.g. toads, frogs, salamanders or newts
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61J—CONTAINERS SPECIALLY ADAPTED FOR MEDICAL OR PHARMACEUTICAL PURPOSES; DEVICES OR METHODS SPECIALLY ADAPTED FOR BRINGING PHARMACEUTICAL PRODUCTS INTO PARTICULAR PHYSICAL OR ADMINISTERING FORMS; DEVICES FOR ADMINISTERING FOOD OR MEDICINES ORALLY; BABY COMFORTERS; DEVICES FOR RECEIVING SPITTLE
- A61J3/00—Devices or methods specially adapted for bringing pharmaceutical products into particular physical or administering forms
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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
- A61K9/0012—Galenical forms characterised by the site of application
- A61K9/0019—Injectable compositions; Intramuscular, intravenous, arterial, subcutaneous administration; Compositions to be administered through the skin in an invasive manner
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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
- A61K9/08—Solutions
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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)
- A61K36/185—Magnoliopsida (dicotyledons)
- A61K36/23—Apiaceae or Umbelliferae (Carrot family), e.g. dill, chervil, coriander or cumin
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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)
- A61K36/185—Magnoliopsida (dicotyledons)
- A61K36/48—Fabaceae or Leguminosae (Pea or Legume family); Caesalpiniaceae; Mimosaceae; Papilionaceae
- A61K36/481—Astragalus (milkvetch)
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Abstract
The invention discloses the filter methods in a kind of Venenum Bufonis Injection preparation process to be soaked in propylene glycol comprising the following specific steps taking 10 ~ 15g of the dried venom of toads, is put into heating room and is dried after taking-up, is ground after the completion of drying；Mixed solution, which is put into refrigerating chamber, carries out chilling treatment, after taking-up, carries out filtering for the first time and second is filtered, first time filter residue and second of filter residue is admixed together, carbon tetrachloride is added, is filtered after stirring and dissolving, heating recovery carbon tetrachloride obtains third time clear liquid and third time filter residue；Merge first time clear liquid, second of clear liquid and third time clear liquid, obtains toad cake extract.
Description
Technical field
The invention belongs to dried venom of toads preparation technical fields, and in particular to the filtering side in a kind of Venenum Bufonis Injection preparation process
Method.
Background technique
The dried venom of toads is processed from strand by the ear rear gland and skin gland secretion object of Bufonidae amphibians faunal, is traditional Chinese medicine
Material.The bioactive substances such as steroidal object, alkaloid contained by the dried venom of toads have the multiple functions such as detoxify, ease pain, having one's ideas straightened out, is antitumor and by
It is widely applied.Taking crisp method is that toad is put into basket, is jiggled in water, after washing away the silt of body surface, draining the water just
Slurry can be scraped.Venenum Bufonis Injection has clearing heat and detoxicating effect, and it is slow can be widely used in the various urgency such as carbuncle swells sore of excessive noxious heat
Property pyogenic infection and the treatment of tumour.In the preparation process of Venenum Bufonis Injection, first has to extract toad cake extract, extract
Filtering in the process can filter out impurity therein, and traditional filter method is exactly simply once to be filtered, filter effect
Difference, product yield is low, in consideration of it, it is necessary to make improvement to the filter method in traditional Venenum Bufonis Injection preparation process.
Summary of the invention
To solve the deficiencies in the prior art, the purpose of the present invention is to provide the mistakes in a kind of Venenum Bufonis Injection preparation process
Filtering method, can be sufficiently and finer and smoother by dried venom of toads grinding, avoids the dried venom of toads from grinding insufficient problem, and can adequately filter out
Impurity, and can avoid the waste for the filtrate carried secretly in filter residue, further increase the yield and degree of purity of product.
In order to achieve the above objectives, the present invention adopts the following technical scheme that:
A kind of filter method in Venenum Bufonis Injection preparation process, comprising the following specific steps
S1,10 ~ 15g of the dried venom of toads is taken, is soaked in 15 ~ 25min in propylene glycol, be put into heating room and dried after taking-up, dried
At rear taking-up, when temperature drops to 30 ~ 35 DEG C, the dried venom of toads is subjected to first time milled processed, after grinding 0.4 ~ 0.8h, then is carried out
Second of milled processed obtains dried venom of toads grounds travel after grinding 0.6 ~ 0.9h, spare；
S2, each component stock based on following parts by weight: 22 ~ 27 parts of dried venom of toads fine powder, 21 ~ 29 parts of ethyl alcohol, 13 ~ 22 parts of Radix Astragali, north
15 ~ 20 parts of the root of straight ladybell, 11 ~ 17 parts of glycerol, 18 ~ 25 parts of disodium ethylene diamine tetraacetate, 14 ~ 19 parts of sodium chloride, anhydrous sodium sulfite 6 ~
13 parts, 8 ~ 11 parts and 16 ~ 22 parts of water of diethylamine；
S3, it said components is put into reaction kettle mixes, stir evenly, 1.5 ~ 2.5h of continuous heating obtains mixing molten
Liquid；
S4, mixed solution, which are put into refrigerating chamber, carries out chilling treatment, after taking-up, carries out first time filtering, takes out upper layer for the first time
Clear liquid collects first time filter residue；
S5, ethyl alcohol is added in obtained first time clear liquid, after mixing evenly, carries out second and filter, heating recovery ethyl alcohol takes
Second of upper layer clear liquid out collects second of filter residue；
It is S6, first time filter residue and second of filter residue is admixed together, carbon tetrachloride is added, filters, heats back after stirring and dissolving
Carbon tetrachloride is received, third time clear liquid and third time filter residue are obtained；
S7, merge first time clear liquid, second of clear liquid and third time clear liquid, obtain toad cake extract.
Preferably, in abovementioned steps S1, the temperature for heating room is 80 ~ 95 DEG C, and heating rate is 8 ~ 13 DEG C/min, when drying
Between be 0.5 ~ 1.3h.
More preferably, in abovementioned steps S1, the dried venom of toads fine powder after first time milled processed is 150 ~ 180 mesh, is ground for the second time
Mill treated dried venom of toads fine powder is 230 ~ 260 mesh.
It is highly preferred that the mixing speed of reaction kettle is 500 ~ 600 turns/min in above mentioned step S3, heating temperature is 55 ~ 65
℃。
It is further preferred that the temperature of refrigerating chamber is 1 ~ 8 DEG C in abovementioned steps S4, cold preservation time is 1.5 ~ 2h.
Specifically, in abovementioned steps S5, the mass ratio of first time clear liquid and ethyl alcohol is (2 ~ 4): (1 ~ 3).
Preferably, in abovementioned steps S6, the quality of the quality sum and carbon tetrachloride of first time filter residue and second filter residue
Than for (2 ~ 5): (2 ~ 3).
The invention has the beneficial effects that: the filter method in Venenum Bufonis Injection preparation process of the invention is easy to operate,
First the dried venom of toads is soaked in propylene glycol, then dries and grinds while hot again twice, can be sufficiently and finer and smoother by dried venom of toads grinding, it keeps away
Exempt from the dried venom of toads and grind insufficient problem, improves the yield of the dried venom of toads；By to the filter residue filtered twice it is for re-filtering after, can
Adequately to filter out impurity, and the yield of product and pure to avoid the waste for the filtrate carried secretly in filter residue, can be further increased
Degree.
Specific embodiment
Below in conjunction with detailed description of the invention by specific embodiments.
Embodiment 1
A kind of filter method in Venenum Bufonis Injection preparation process, comprising the following specific steps
S1, dried venom of toads 10g is taken, is soaked in 15min in propylene glycol, be put into heating room and dried after taking-up, heat the temperature in room
It is 80 DEG C, heating rate is 8 DEG C/min, drying time 0.5h, is taken out after the completion of drying, will when temperature drops to 30 DEG C
The dried venom of toads carries out first time milled processed, and dried venom of toads fine powder is 150 mesh after grinding 0.4h, then carries out second of milled processed, grinds
Dried venom of toads fine powder is 230 mesh after 0.6h, obtains dried venom of toads grounds travel, spare；
S2, based on following parts by weight each component stock: 22 parts of dried venom of toads fine powder, 21 parts of ethyl alcohol, 13 parts of Radix Astragali, 15 parts of Radix Glehniae,
11 parts of glycerol, 18 parts of disodium ethylene diamine tetraacetate, 14 parts of sodium chloride, 6 parts of anhydrous sodium sulfite, 8 parts of diethylamine and 16 parts of water；
S3, it said components is put into reaction kettle mixes, stir evenly, mixing speed is 500 turns/min, heating temperature
It is 55 DEG C, continuous heating 1.5h obtains mixed solution；
S4, mixed solution, which are put into refrigerating chamber, carries out chilling treatment, and refrigerated storage temperature is 1 DEG C, cold preservation time 1.5h, after taking-up,
First time filtering is carried out, upper layer first time clear liquid is taken out, collects first time filter residue；
S5, it is added ethyl alcohol in obtained first time clear liquid, the mass ratio of first time clear liquid and ethyl alcohol is 2:1, after mixing evenly,
It carries out second to filter, heating recovery ethyl alcohol takes out second of upper layer clear liquid, collects second of filter residue；
S6, first time filter residue and second of filter residue is admixed together, addition carbon tetrachloride, first time filter residue and second of filter residue
Quality sum and the mass ratio of carbon tetrachloride be 2:2, filter after stirring and dissolving, heating recovery carbon tetrachloride, obtain third time
Clear liquid and third time filter residue；
S7, merge first time clear liquid, second of clear liquid and third time clear liquid, obtain toad cake extract.
Embodiment 2
A kind of filter method in Venenum Bufonis Injection preparation process, comprising the following specific steps
S1, dried venom of toads 15g is taken, is soaked in 25min in propylene glycol, be put into heating room and dried after taking-up, heat the temperature in room
It is 95 DEG C, heating rate is 13 DEG C/min, drying time 1.3h, is taken out after the completion of drying, will when temperature drops to 35 DEG C
The dried venom of toads carries out first time milled processed, and dried venom of toads fine powder is 180 mesh after grinding 0.8h, then carries out second of milled processed, grinds
Dried venom of toads fine powder is 260 mesh after 0.9h, obtains dried venom of toads grounds travel, spare；
S2, based on following parts by weight each component stock: 27 parts of dried venom of toads fine powder, 29 parts of ethyl alcohol, 22 parts of Radix Astragali, 20 parts of Radix Glehniae,
17 parts of glycerol, 25 parts of disodium ethylene diamine tetraacetate, 19 parts of sodium chloride, 13 parts of anhydrous sodium sulfite, 11 parts of diethylamine and 22 parts of water；
S3, it said components is put into reaction kettle mixes, stir evenly, mixing speed is 600 turns/min, heating temperature
It is 65 DEG C, continuous heating 2.5h obtains mixed solution；
S4, mixed solution, which are put into refrigerating chamber, carries out chilling treatment, and refrigerated storage temperature is 8 DEG C, cold preservation time 2h, after taking-up, into
Row filters for the first time, takes out upper layer first time clear liquid, collects first time filter residue；
S5, it is added ethyl alcohol in obtained first time clear liquid, the mass ratio of first time clear liquid and ethyl alcohol is 4:3, after mixing evenly,
It carries out second to filter, heating recovery ethyl alcohol takes out second of upper layer clear liquid, collects second of filter residue；
S6, first time filter residue and second of filter residue is admixed together, addition carbon tetrachloride, first time filter residue and second of filter residue
Quality sum and the mass ratio of carbon tetrachloride be 5:3, filter after stirring and dissolving, heating recovery carbon tetrachloride, obtain third time
Clear liquid and third time filter residue；
S7, merge first time clear liquid, second of clear liquid and third time clear liquid, obtain toad cake extract.
Embodiment 3
A kind of filter method in Venenum Bufonis Injection preparation process, comprising the following specific steps
S1, dried venom of toads 12g is taken, is soaked in 20min in propylene glycol, be put into heating room and dried after taking-up, heat the temperature in room
It is 85 DEG C, heating rate is 11 DEG C/min, drying time 1h, is taken out after the completion of drying, when temperature drops to 32 DEG C, by toad
Shortcake carries out first time milled processed, and dried venom of toads fine powder is 170 mesh after grinding 0.6h, then carries out second of milled processed, grinds 0.8h
Dried venom of toads fine powder is 250 mesh afterwards, obtains dried venom of toads grounds travel, spare；
S2, based on following parts by weight each component stock: 25 parts of dried venom of toads fine powder, 25 parts of ethyl alcohol, 17 parts of Radix Astragali, 18 parts of Radix Glehniae,
14 parts of glycerol, 21 parts of disodium ethylene diamine tetraacetate, 16 parts of sodium chloride, 10 parts of anhydrous sodium sulfite, 9 parts of diethylamine and 19 parts of water；
S3, it said components is put into reaction kettle mixes, stir evenly, mixing speed is 550 turns/min, heating temperature
It is 60 DEG C, continuous heating 2h obtains mixed solution；
S4, mixed solution, which are put into refrigerating chamber, carries out chilling treatment, and refrigerated storage temperature is 5 DEG C, cold preservation time 1.8h, after taking-up,
First time filtering is carried out, upper layer first time clear liquid is taken out, collects first time filter residue；
S5, it is added ethyl alcohol in obtained first time clear liquid, the mass ratio of first time clear liquid and ethyl alcohol is 3:2, after mixing evenly,
It carries out second to filter, heating recovery ethyl alcohol takes out second of upper layer clear liquid, collects second of filter residue；
S6, first time filter residue and second of filter residue is admixed together, addition carbon tetrachloride, first time filter residue and second of filter residue
Quality sum and the mass ratio of carbon tetrachloride be 3:3, filter after stirring and dissolving, heating recovery carbon tetrachloride, obtain third time
Clear liquid and third time filter residue；
S7, merge first time clear liquid, second of clear liquid and third time clear liquid, obtain toad cake extract.
The basic principles, main features and advantages of the invention have been shown and described above.The technical staff of the industry should
Understand, the above embodiments do not limit the invention in any form, all obtained by the way of equivalent substitution or equivalent transformation
Technical solution is fallen within the scope of protection of the present invention.
Claims (7)
1. the filter method in a kind of Venenum Bufonis Injection preparation process, which is characterized in that comprising the following specific steps
S1,10 ~ 15g of the dried venom of toads is taken, is soaked in 15 ~ 25min in propylene glycol, be put into heating room and dried after taking-up, dried
At rear taking-up, when temperature drops to 30 ~ 35 DEG C, the dried venom of toads is subjected to first time milled processed, after grinding 0.4 ~ 0.8h, then is carried out
Second of milled processed obtains dried venom of toads grounds travel after grinding 0.6 ~ 0.9h, spare；
S2, each component stock based on following parts by weight: 22 ~ 27 parts of dried venom of toads fine powder, 21 ~ 29 parts of ethyl alcohol, 13 ~ 22 parts of Radix Astragali, north
15 ~ 20 parts of the root of straight ladybell, 11 ~ 17 parts of glycerol, 18 ~ 25 parts of disodium ethylene diamine tetraacetate, 14 ~ 19 parts of sodium chloride, anhydrous sodium sulfite 6 ~
13 parts, 8 ~ 11 parts and 16 ~ 22 parts of water of diethylamine；
S3, it said components is put into reaction kettle mixes, stir evenly, 1.5 ~ 2.5h of continuous heating obtains mixing molten
Liquid；
S4, mixed solution, which are put into refrigerating chamber, carries out chilling treatment, after taking-up, carries out first time filtering, takes out upper layer for the first time
Clear liquid collects first time filter residue；
S5, ethyl alcohol is added in obtained first time clear liquid, after mixing evenly, carries out second and filter, heating recovery ethyl alcohol takes
Second of upper layer clear liquid out collects second of filter residue；
It is S6, first time filter residue and second of filter residue is admixed together, carbon tetrachloride is added, filters, heats back after stirring and dissolving
Carbon tetrachloride is received, third time clear liquid and third time filter residue are obtained；
S7, merge first time clear liquid, second of clear liquid and third time clear liquid, obtain toad cake extract.
2. the filter method in a kind of Venenum Bufonis Injection preparation process according to claim 1, which is characterized in that the step
In rapid S1, the temperature for heating room is 80 ~ 95 DEG C, and heating rate is 8 ~ 13 DEG C/min, and drying time is 0.5 ~ 1.3h.
3. the filter method in a kind of Venenum Bufonis Injection preparation process according to claim 1, which is characterized in that the step
In rapid S1, the dried venom of toads fine powder after first time milled processed is 150 ~ 180 mesh, and the dried venom of toads fine powder after second of milled processed is
230 ~ 260 mesh.
4. the filter method in a kind of Venenum Bufonis Injection preparation process according to claim 1, which is characterized in that the step
In rapid S3, the mixing speed of reaction kettle is 500 ~ 600 turns/min, and heating temperature is 55 ~ 65 DEG C.
5. the filter method in a kind of Venenum Bufonis Injection preparation process according to claim 1, which is characterized in that the step
In rapid S4, the temperature of refrigerating chamber is 1 ~ 8 DEG C, and cold preservation time is 1.5 ~ 2h.
6. the filter method in a kind of Venenum Bufonis Injection preparation process according to claim 1, which is characterized in that the step
In rapid S5, the mass ratio of first time clear liquid and ethyl alcohol is (2 ~ 4): (1 ~ 3).
7. the filter method in a kind of Venenum Bufonis Injection preparation process according to claim 1, which is characterized in that the step
In rapid S6, the mass ratio of the quality sum and carbon tetrachloride of first time filter residue and second filter residue is (2 ~ 5): (2 ~ 3).
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Cited By (1)
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| CN109464469A (en) * | 2018-10-19 | 2019-03-15 | 江苏浦金药业有限公司 | A kind of extracting method of the dried venom of toads |
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Application publication date: 20190122 |
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