CN106619836A - Method for extracting active ingredient from all-grass of Bothriospermum chinense Bunge and applications of active ingredient - Google Patents
Method for extracting active ingredient from all-grass of Bothriospermum chinense Bunge and applications of active ingredient Download PDFInfo
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- CN106619836A CN106619836A CN201611016203.5A CN201611016203A CN106619836A CN 106619836 A CN106619836 A CN 106619836A CN 201611016203 A CN201611016203 A CN 201611016203A CN 106619836 A CN106619836 A CN 106619836A
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- homoplantaginin
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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)
- A61K36/68—Plantaginaceae (Plantain Family)
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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
- A61K2236/10—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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- 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
- A61K2236/19—Preparation or pretreatment of starting material involving fermentation using yeast, bacteria or both; enzymatic treatment
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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
- A61K2236/33—Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones
- A61K2236/333—Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones using mixed solvents, e.g. 70% EtOH
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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
- A61K2236/51—Concentration or drying of the extract, e.g. Lyophilisation, freeze-drying or spray-drying
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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 discloses a method for extracting an active ingredient from all-grass of Bothriospermum chinense Bunge and applications of the active ingredient. The method comprises the following steps: drying, grinding, crude extraction and refining; the obtained product is high in purity and high in yield; when the obtained homoplantaginin is used for treating a pregnant sow suffering from low fever, the effect is obvious, and meanwhile, no influences are caused to the fetus in the belly of the sow.
Description
Technical field
The present invention relates to pharmaceutical technology field, and in particular to the extracting method of effective ingredient and its should in a kind of Bufo siccuss grass
With.
Background technology
Bufo siccuss grass is a kind of upright draft, high 15～19cm, multi-branched.Be it is a kind of it is wild, than sparser Chinese herbal medicine.
It can effectively prevent and treat the diseases such as flu, chronic enteritiss, have significant effect to treatment cough and bronchitis.Bufo siccuss
Grass is dwelt the preventing and treating of reptile Bufo siccuss secretions Venenum Bufonis and the Cutis Bufonis containing such material, toad-cortex, Bufo siccus in some diseases with two
Aspect, what is played the same tune on different musical instruments is wonderful.
Effective ingredient in Bufo siccuss grass is mainly homoplantaginin, and homoplantaginin is mainly used at present the bronchus for the treatment of people
Inflammation, its toxicity is less.But it is less currently for the Study on Extraction Method of effective ingredient in Bufo siccuss grass, it is badly in need of a kind of simple
And can obtain the extracting method of high level homoplantaginin.
There are the symptoms such as low grade fever, inappetence in pregnancy, often in sow, if now using common drug treatment to it,
It is easy to damage the fetus in its tripe, the generation of dead fetuses by abortion aged phenomenon can be caused when serious.Therefore it is badly in need of a kind of science
Administrated method solving the symptom of in-pig low grade fever.
The content of the invention
In order to solve the above problems, the invention provides a kind of Bufo siccuss grass in effective ingredient extracting method and its treatment
Application in terms of sow low grade fever.
The present invention is achieved by the following technical solutions.
A kind of extracting method of effective ingredient in Bufo siccuss grass, extraction is comprised the following steps：
（1）Drying grinds：The Bufo siccuss grass Herb of growth and maturity is taken, is put in dehydrator and is dried, drying temperature is set as 50-60
DEG C, drying time is 30-40min, and the Bufo siccuss grass meal after drying is broken to into 80-100 mesh；
（2）Slightly carry：Bufo siccuss grass after crushing is put in container, and is added thereto to the distilled water of 10-15 times of quality weight, will be steamed
Distilled water is heated to 35-37 DEG C, is then added thereto to mixing enzyme preparation, filters to obtain filtering residue after stirring 30-50min, then by filtering residue
In being put into the distilled water of 15-20 times of quality weight, and the sulfuric acid solution that volume fraction is 15% is added thereto to, adjusts the pH of solution
To 2.8-3.0, then solution is heated to into 100 DEG C, is cooled after extraction 3-4 hours, during extraction, persistently with ultrasound
Process, then filter in the mixture for obtaining, the filtrate for obtaining is put in 3-5 DEG C of environment to be lowered the temperature, and cooling processes 2-3 hours
Afterwards, filtered again, the homoplantaginin crude product for obtaining；Bufo siccuss grass after being crushed using mixing enzyme preparation process, can be by toad
Lipid and cellulose decomposition in bufonid toad grass roots stem for small molecule material, reduce in these macromolecular complex confrontation Bufo siccuss grass effectively into
The adsorption for dividing, so as in extraction, can rapidly and thoroughly extract the effective ingredient in Bufo siccuss grass；Will with concentrated sulphuric acid
The pH regulator of solution uses supersound process to 2.8-3.0, is conducive to homoplantaginin to separate out from Bufo siccuss grass, improves the receipts of product
Rate；
（3）Refine：By step（2）In the ethanol solution of the dissolving crude product 95% of gained, concentration is added in solution for 20-25%'s
Ammonia, adjusts the pH to 8.0-8.5 of solution, Rotary Evaporators concentrating under reduced pressure is then used, after 1.0-1.5 hours, by the crystalline substance for obtaining
Body material is dissolved in again in 100 DEG C of distilled water, is lowered the temperature in the environment of then solution being put into into 1-3 DEG C, is recrystallized to give height
Plantagin fine work；Now by the pH regulator of solution to alkalescence, stability of the homoplantaginin in concentration can be increased, be prevented dense
As ethanol solution is distributed together during contracting, wherein Rotary Evaporators are purchased from Shanghai Peng Ming biotechnologies Development Co., Ltd,
Specification is 50L；
The homoplantaginin extracted from Bufo siccuss grass is made into tablet as sole active ingredient, wherein high contained by every tablet
Plantagin 2-3g, uses when low grade fever occurs in in-pig, and using method is as follows：After low grade fever occurs in in-pig, by 1-2 grains
Tablet is put in sow feed, is respectively administered once sooner or later daily, successive administration two days；Homoplantaginin can effectively treat pregnant mother
Low grade fever's symptom of pig, and the fetus in sow tripe is not damaged, general medication two days, sow low grade fever can decorporate.
Above-mentioned steps（2）Described in mixing enzyme preparation be made up of the component of following weight portion：Cellulase 10-15 parts,
Lipase 8-10 parts.
Beneficial effect：The extracting method of effective ingredient and its application, the work of extraction in a kind of Bufo siccuss grass that the present invention is provided
Skill is simple, materials environmental protection, and the yield of homoplantaginin and purity are high；Homoplantaginin is made into tablet, for treating in-pig
Low grade fever, will not have any impact to the fetus in sow body, and drug effect is fast, and low grade fever sow can be made quickly to bring down a fever.
Specific implementation method
Embodiment 1
A kind of extracting method of effective ingredient in Bufo siccuss grass, extraction is comprised the following steps：
（1）Drying grinds：The Bufo siccuss grass Herb of growth and maturity is taken, is put in dehydrator and is dried, drying temperature is set as 50 DEG C, dries
The dry time is 30min, and the Bufo siccuss grass meal after drying is broken to into 80 mesh；
（2）Slightly carry：Bufo siccuss grass after crushing is put in container, and is added thereto to the distilled water of 10 times of quality weights, will be distilled
Water is heated to 35 DEG C, is then added thereto to mixing enzyme preparation, and after stirring 30min filtering residue is filtered to obtain, then filtering residue is put into into 15 times
In the distilled water of quality weight, and the sulfuric acid solution that volume fraction is 15% is added thereto to, adjusts the pH to 2.8 of solution, then will
Solution is heated to 100 DEG C, extraction cools after 3 hours, during extraction, persistently with supersound process, then will obtain
Mixture is filtered, and the filtrate for obtaining is put in 3 DEG C of environment to be lowered the temperature, and after cooling is processed 2 hours, is filtered again, is obtained
Homoplantaginin crude product；
（3）Refine：By step（2）In the ethanol solution of the dissolving crude product 95% of gained, the ammonia that concentration is 20% is added in solution
Water, adjusts the pH to 8.0 of solution, then uses Rotary Evaporators concentrating under reduced pressure, after 1.0 hours, by the crystalline solid for obtaining again
In being dissolved in 100 DEG C of distilled water, lower the temperature in the environment of then solution being put into into 1 DEG C, be recrystallized to give homoplantaginin fine work.
The homoplantaginin extracted from Bufo siccuss grass is made into tablet as sole active ingredient, wherein every tablet institute
2-3g containing homoplantaginin, uses when low grade fever occurs in in-pig, and using method is as follows：After low grade fever occurs in in-pig, by 1
Grain tablet is put in sow feed, is respectively administered once sooner or later daily, successive administration two days.
Step（2）Described in mixing enzyme preparation be made up of the component of following weight portion：10 parts of cellulase, lipase 8
Part.
In the present embodiment, the yield of homoplantaginin is 87.4%, and purity is 99.3%.
Embodiment 2
A kind of extracting method of effective ingredient in Bufo siccuss grass, extraction is comprised the following steps：
（1）Drying grinds：The Bufo siccuss grass Herb of growth and maturity is taken, is put in dehydrator and is dried, drying temperature is set as 55 DEG C, dries
The dry time is 35min, and the Bufo siccuss grass meal after drying is broken to into 90 mesh；
（2）Slightly carry：Bufo siccuss grass after crushing is put in container, and is added thereto to the distilled water of 13 times of quality weights, will be distilled
Water is heated to 36 DEG C, is then added thereto to mixing enzyme preparation, and after stirring 40min filtering residue is filtered to obtain, then filtering residue is put into into 17 times
In the distilled water of quality weight, and the sulfuric acid solution that volume fraction is 15% is added thereto to, adjusts the pH to 2.8-3.0 of solution, so
Afterwards solution is heated to into 100 DEG C, extraction cools after 3.5 hours, during extraction, persistently with supersound process, then will
The mixture for obtaining is filtered, and the filtrate for obtaining is put in 4 DEG C of environment to be lowered the temperature, and after cooling is processed 2.5 hours, is carried out again
Filter, the homoplantaginin crude product for obtaining；
（3）Refine：By step（2）In the ethanol solution of the dissolving crude product 95% of gained, the ammonia that concentration is 22% is added in solution
Water, adjusts the pH to 8.4 of solution, then uses Rotary Evaporators concentrating under reduced pressure, after 1.3 hours, by the crystalline solid for obtaining again
In being dissolved in 100 DEG C of distilled water, lower the temperature in the environment of then solution being put into into 2 DEG C, be recrystallized to give homoplantaginin fine work.
The homoplantaginin extracted from Bufo siccuss grass is made into tablet as sole active ingredient, wherein every tablet institute
2.5g containing homoplantaginin, uses when low grade fever occurs in in-pig, and using method is as follows：After low grade fever occurs in in-pig, by 1
Grain tablet is put in sow feed, is respectively administered once sooner or later daily, successive administration two days.
Step（2）Described in mixing enzyme preparation be made up of the component of following weight portion：13 parts of cellulase, lipase 9
Part.
In the present embodiment, the yield of homoplantaginin is 88.1%, and purity is 99.4%.
Embodiment 3
A kind of extracting method of effective ingredient in Bufo siccuss grass, extraction is comprised the following steps：
（1）Drying grinds：The Bufo siccuss grass Herb of growth and maturity is taken, is put in dehydrator and is dried, drying temperature is set as 60 DEG C, dries
The dry time is 40min, and the Bufo siccuss grass meal after drying is broken to into 100 mesh；
（2）Slightly carry：Bufo siccuss grass after crushing is put in container, and is added thereto to the distilled water of 15 times of quality weights, will be distilled
Water is heated to 37 DEG C, is then added thereto to mixing enzyme preparation, and after stirring 50min filtering residue is filtered to obtain, then filtering residue is put into into 20 times
In the distilled water of quality weight, and the sulfuric acid solution that volume fraction is 15% is added thereto to, adjusts the pH to 3.0 of solution, then will
Solution is heated to 100 DEG C, extraction cools after 4 hours, during extraction, persistently with supersound process, then will obtain
Mixture is filtered, and the filtrate for obtaining is put in 5 DEG C of environment to be lowered the temperature, and after cooling is processed 3 hours, is filtered again, is obtained
Homoplantaginin crude product；
（3）Refine：By step（2）In the ethanol solution of the dissolving crude product 95% of gained, the ammonia that concentration is 25% is added in solution
Water, adjusts the pH to 8.5 of solution, then uses Rotary Evaporators concentrating under reduced pressure, after 1.5 hours, by the crystalline solid for obtaining again
In being dissolved in 100 DEG C of distilled water, lower the temperature in the environment of then solution being put into into 3 DEG C, be recrystallized to give homoplantaginin fine work.
The homoplantaginin extracted from Bufo siccuss grass is made into tablet as sole active ingredient, wherein every tablet institute
3g containing homoplantaginin, uses when low grade fever occurs in in-pig, and using method is as follows：After low grade fever occurs in in-pig, by 2
Tablet is put in sow feed, is respectively administered once sooner or later daily, successive administration two days.
Step（2）Described in mixing enzyme preparation be made up of the component of following weight portion：15 parts of cellulase, lipase 10
Part.
In the present embodiment, the yield of homoplantaginin is 88.1%, and purity is 99.6%.
Test：
By the way of embodiment 1, in Feixi County, plant is tested in-pig, finds the gestation to low grade fever
Sow, this product treatment is evident in efficacy, and in-pig can bring down a fever completely for second day after medication, and to the tire in the tripe of sow
Youngster does not produce any impact, and does not affect the fertility of sow.
Claims (3)
1. the extracting method of effective ingredient during a kind of Bufo siccuss are careless, it is characterised in that extraction is comprised the following steps：
Drying grinds：The Bufo siccuss grass Herb of growth and maturity is taken, is put in dehydrator and is dried, drying temperature is set as 50-60 DEG C, dries
The dry time is 30-40min, and the Bufo siccuss grass meal after drying is broken to into 80-100 mesh；
Slightly carry：Bufo siccuss grass after crushing is put in container, and is added thereto to the distilled water of 10-15 times of quality weight, will be distilled
Water is heated to 35-37 DEG C, is then added thereto to mixing enzyme preparation, and after stirring 30-50min filtering residue is filtered to obtain, then filtering residue is put
In entering the distilled water of 15-20 times of quality weight, and be added thereto to the sulfuric acid solution that volume fraction is 15%, adjust the pH of solution to
2.8-3.0, is then heated to 100 DEG C by solution, cools after extraction 3-4 hours, during extraction, persistently uses at ultrasound
Reason, then filters in the mixture for obtaining, and the filtrate for obtaining is put in 3-5 DEG C of environment to be lowered the temperature, and cooling is processed after 2-3 hours,
Filtered again, the homoplantaginin crude product for obtaining；
Refine：By step（2）In the ethanol solution of the dissolving crude product 95% of gained, concentration is added in solution for the ammonia of 20-25%
Water, adjusts the pH to 8.0-8.5 of solution, Rotary Evaporators concentrating under reduced pressure is then used, after 1.0-1.5 hours, by the crystal for obtaining
Material is dissolved in again in 100 DEG C of distilled water, is lowered the temperature in the environment of then solution being put into into 1-3 DEG C, is recrystallized to give high car
Front glycoside fine work.
2. the application of effective ingredient during a kind of Bufo siccuss are careless, it is characterised in that make the homoplantaginin extracted from Bufo siccuss grass
Tablet is made for sole active ingredient, wherein homoplantaginin 2-3g contained by every tablet, uses when low grade fever occurs in in-pig,
Using method is as follows：After low grade fever occurs in in-pig, 1-2 grain tablets are put in sow feed, daily each administration one sooner or later
It is secondary, successive administration two days.
3. according to the extracting method of effective ingredient in a kind of Bufo siccuss grass described in claim 1, it is characterised in that step（2）
Described in mixing enzyme preparation be made up of the component of following weight portion：Cellulase 10-15 parts, lipase 8-10 parts.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611016203.5A CN106619836A (en) | 2016-11-18 | 2016-11-18 | Method for extracting active ingredient from all-grass of Bothriospermum chinense Bunge and applications of active ingredient |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201611016203.5A CN106619836A (en) | 2016-11-18 | 2016-11-18 | Method for extracting active ingredient from all-grass of Bothriospermum chinense Bunge and applications of active ingredient |
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| CN106619836A true CN106619836A (en) | 2017-05-10 |
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Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105816521A (en) * | 2016-06-03 | 2016-08-03 | 陈瑞 | Bothriospermum chinense (Turcz.) bunge extract for treating urinary tract infection |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105816521A (en) * | 2016-06-03 | 2016-08-03 | 陈瑞 | Bothriospermum chinense (Turcz.) bunge extract for treating urinary tract infection |
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