CN106432402A - Extraction process of cinobufagin extract - Google Patents
Extraction process of cinobufagin extract Download PDFInfo
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- CN106432402A CN106432402A CN201610848800.8A CN201610848800A CN106432402A CN 106432402 A CN106432402 A CN 106432402A CN 201610848800 A CN201610848800 A CN 201610848800A CN 106432402 A CN106432402 A CN 106432402A
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07J—STEROIDS
- C07J71/00—Steroids in which the cyclopenta(a)hydrophenanthrene skeleton is condensed with a heterocyclic ring
- C07J71/0005—Oxygen-containing hetero ring
- C07J71/001—Oxiranes
- C07J71/0021—Oxiranes at position 14(15)
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Abstract
The invention discloses an extraction process of cinobufagin extract. The extraction process mainly comprises the following steps that toad skin is boiled twice after being cleaned, filtering is carried out, first alcohol precipitation is carried out after concentration, second alcohol precipitation is carried out after second concentration, ethyl alcohol is recycled till the solution is free of alcohol taste, extract collecting is carried out, finally the finished product is prepared, and the finished product is refrigerated. The cinobufagin extract is prepared through the processes of boiling, filtering, concentration, alcohol precipitation and the like of the toad skin, the preparation process is simple, operation is easy, and the prepared extract contains fewer impurities, is high in purity and high in extraction rate and has very high application value.
Description
Technical field
The present invention relates to technical field of Chinese medicines, especially a kind of extraction process of Cinobufacini extract.
Background technology
The skin that cinobufacin (Cutis Bufonis) extract derives from Bufo siccus obtains through extracting to separate.Cancer patient is in China
Or even whole world sickness rate and mortality rate all very high, China cancer patient presses 9,000,000 people (sickness rate press 7 ‰) and calculates, then plus often
Year increases 1,000,000 people, nearly 10,000,000 people of cancer patient's number newly.Cancer patient is once found, and most is middle and advanced stage, from
It is found to death averagely at 12-18 month.At present, widely used Therapeutic Method is chemical medicinal treatment, these methods
It is accompanied by seriously toxicity, or even make patient's immunity degradation it is impossible to reach preferable therapeutic effect.Therefore,
Study and find exploitation from Chinese medicine and there is the low tcm product of notable anti-tumor activity, toxic and side effects, become in this field solely
Special, to have innovative significance means and invention, its application prospect is very wide.
Content of the invention
The technical problem to be solved is to provide a kind of extraction process of Cinobufacini extract.
For solving above-mentioned technical problem, the technical solution used in the present invention is：A kind of extraction process of Cinobufacini extract,
Comprise the following steps：
1) Cutis Bufonis after taking 1 weight portion to clean, add the water of 3-10 parts by volume, use strainer filtering after decocting 30-60 minute,
Obtain filtrate 1 and filtering residue 1；
2) add the water of 2-6 parts by volume in described filtering residue 1, use strainer filtering after decocting 20-40 minute, obtain filtrate 2
With filtering residue 2；
3) by 2-in-1 to described filtrate 1 and filtrate and after be placed in concentration tank concentrate, obtain concentrated solution 1 after concentration；
4) add ethanol in described concentrated solution 1, the alcohol content adjusting concentrated solution, to 50-75%, stands after stirring
24-72 hour, inclines and takes its supernatant to obtain supernatant 1；
5) take described step 4) supernatant 1 that obtains, obtain concentrated solution 2 after concentration and recovery ethanol to its no alcohol taste；
6) add ethanol in the concentrated solution 2 being obtained to described step 5, adjust its alcohol content to 70-95%, stir
Stand 36-48 hour afterwards, incline and take its supernatant to obtain supernatant 2；
7) take described step 5) supernatant 2 that obtains, carry out after concentration and recovery ethanol to its no alcohol taste receiving cream, China toad is obtained
Extract, and cold preservation.
Preferably, a kind of extraction process of Cinobufacini extract, comprises the following steps：
1) Cutis Bufonis after taking 1 weight portion to clean, add the water of 8 parts by volume, with the strainer filtering of 60 mesh after decocting 45 minutes,
Obtain filtrate 1 and filtering residue 1；
2) add the water of 4 parts by volume in described filtering residue 1, with the strainer filtering of 60 mesh after decocting 30 minutes, obtain filtrate 2
With filtering residue 2；
3) by 2-in-1 to described filtrate 1 and filtrate and after be placed in concentration tank concentrate, obtain concentrated solution after concentration；
4) add ethanol in described concentrated solution, the alcohol content adjusting concentrated solution, to 70%, stands 72 little after stirring
When, incline and take its supernatant to obtain supernatant 1；
5) take described step 4) supernatant 1 that obtains, obtain concentrated solution 2 after concentration and recovery ethanol to its no alcohol taste；
6) add ethanol in the concentrated solution 2 being obtained to described step 5, adjust its alcohol content to 90%, after stirring
Standing 48 hours, inclines and takes its supernatant to obtain supernatant 2；
7) take described step 5) supernatant 2 that obtains, carry out after concentration and recovery ethanol to its no alcohol taste receiving cream, China toad is obtained
Extract, and cold preservation.
Preferably, described step 1) and step 2) in filter screen filter pore size be 60 mesh.
Preferably, described step 3) in, control concentration process in temperature be 60 DEG C～85 DEG C, vacuum be-
0.06Mpa～-0.09Mpa；Described step 4) in, control the temperature in course of reaction to be 0 DEG C～10 DEG C.
Preferably, described step 5) in, control vacuum in concentration process to be -0.06Mpa～-0.09Mpa, control dense
Temperature in compression process is that 40 DEG C～50 DEG C gradients are incremented to final temperature for 55 DEG C～60 DEG C by initial temperature.
Preferably, described step 6) in, control the temperature in course of reaction to be 0 DEG C～10 DEG C.
Preferably, described step 7) in, control the vacuum in concentration process to be -0.06Mpa～-0.09Mpa, control
Temperature in concentration process is that 40 DEG C～50 DEG C gradients are incremented to final temperature for 55 DEG C～60 DEG C by initial temperature, controls cold preservation
Temperature be -2 DEG C～4 DEG C..
The present invention also provides the Cinobufacini extract prepared by a kind of extraction process by above-mentioned Cinobufacini extract in note
Penetrate the application in liquid, tablet, oral liquid, granule, powder, capsule, pill, soft capsule, ointment, nasal drop and suppository.
Beneficial effects of the present invention：The Cinobufacini extract of the present invention is by Cutis Bufonis through works such as decoction, filtration, concentration, precipitate with ethanol
Skill is obtained, and, it is easy to operation, in obtained extract, impurity content is few for preparation process is simple, and the purity of extract is high, extraction ratio
High, there is very high using value.
Specific embodiment
The present invention is described in further detail below, with make those skilled in the art with reference to specification word being capable of evidence
To implement.
It should be appreciated that used herein such as " have ", "comprising" and " inclusion " term do not allot one or many
The presence of individual other element or a combination thereof or interpolation.
Embodiment 1
A kind of extraction process of Cinobufacini extract, comprises the following steps：
1) Cutis Bufonis after taking 250kg to clean, add 2m3Water, with the strainer filtering of 60 mesh after decocting 45 minutes, filtered
Liquid 1 and filtering residue 1；
2) add 1m in described filtering residue 13Water, with the strainer filtering of 60 mesh after decocting 30 minutes, obtain filtrate 2 and filter
Slag 2；
3) by 2-in-1 to described filtrate 1 and filtrate and after be placed in concentration tank concentrate, control concentration process in temperature be 80
DEG C, vacuum be -0.09Mpa, obtain concentrated solution after concentration；
4) add ethanol in described concentrated solution, the alcohol content adjusting concentrated solution, to 70%, stands 72 little after stirring
When, incline and take its supernatant to obtain supernatant 1；
5) take described step 4) supernatant 1 that obtains, obtain concentrated solution 2 after concentration and recovery ethanol to its no alcohol taste；
6) add ethanol in the concentrated solution 2 being obtained to described step 5, adjust its alcohol content to 90%, after stirring
Standing 48 hours, inclines and takes its supernatant to obtain supernatant 2；
7) take described step 5) supernatant 2 that obtains, carry out after concentration and recovery ethanol to its no alcohol taste receiving cream, China toad is obtained
Extract, and cold preservation.
Wherein, described step 4) in, the temperature during control precipitate with ethanol is 10 DEG C.
Wherein, described step 5) in, control vacuum in concentration process to be -0.09Mpa, control the temperature in concentration process
It is that 40 DEG C of gradients are incremented to final temperature for 55 DEG C by initial temperature.
Wherein, described step 6) in, the temperature during control precipitate with ethanol is 10 DEG C.
Wherein, described step 7) in, control the vacuum in concentration process to be -0.09Mpa, control the temperature in concentration process
Degree is that 40 DEG C of gradients are incremented to final temperature for 60 DEG C by initial temperature, controls the temperature of cold preservation to be -2 DEG C.
Embodiment 2
A kind of extraction process of Cinobufacini extract, comprises the following steps：
1) Cutis Bufonis after taking 200kg to clean, add 1.6m3Water, with the strainer filtering of 60 mesh after decocting 40 minutes, obtain
Filtrate 1 and filtering residue 1；
2) add 0.8m in described filtering residue 13Water, with the strainer filtering of 60 mesh after decocting 25 minutes, obtain filtrate 2 He
Filtering residue 2；
3) by 2-in-1 to described filtrate 1 and filtrate and after be placed in concentration tank concentrate, control concentration process in temperature be 75
DEG C, vacuum be -0.08Mpa, obtain concentrated solution after concentration；
4) add ethanol in described concentrated solution, the alcohol content adjusting concentrated solution, to 65%, stands 72 little after stirring
When, incline and take its supernatant to obtain supernatant 1；
5) take described step 4) supernatant 1 that obtains, obtain concentrated solution 2 after concentration and recovery ethanol to its no alcohol taste；
6) add ethanol in the concentrated solution 2 being obtained to described step 5, adjust its alcohol content to 85%, after stirring
Standing 48 hours, inclines and takes its supernatant to obtain supernatant 2；
7) take described step 5) supernatant 2 that obtains, carry out after concentration and recovery ethanol to its no alcohol taste receiving cream, China toad is obtained
Extract, and cold preservation.
Wherein, described step 4) in, the temperature during control precipitate with ethanol is 5 DEG C.
Wherein, described step 5) in, control vacuum in concentration process to be -0.08Mpa, control the temperature in concentration process
It is that 45 DEG C of gradients are incremented to final temperature for 60 DEG C by initial temperature.
Wherein, described step 6) in, the temperature during control precipitate with ethanol is 5 DEG C.
Wherein, described step 7) in, control the vacuum in concentration process to be -0.08Mpa, control the temperature in concentration process
Degree is that 45 DEG C of gradients are incremented to final temperature for 60 DEG C by initial temperature, control the temperature of cold preservation to be -2 DEG C.
Embodiment 3
A kind of extraction process of Cinobufacini extract, comprises the following steps：
1) Cutis Bufonis after taking 300kg to clean, add 2.4m3Water, with the strainer filtering of 80 mesh after decocting 50 minutes, obtain
Filtrate 1 and filtering residue 1；
2) add 1.2m in described filtering residue 13Water, with the strainer filtering of 80 mesh after decocting 35 minutes, obtain filtrate 2 He
Filtering residue 2；
3) by 2-in-1 to described filtrate 1 and filtrate and after be placed in concentration tank concentrate, control concentration process in temperature be 85
DEG C, vacuum be -0.08Mpa, obtain concentrated solution after concentration；
4) add ethanol in described concentrated solution, the alcohol content adjusting concentrated solution, to 75%, stands 72 little after stirring
When, incline and take its supernatant to obtain supernatant 1；
5) take described step 4) supernatant 1 that obtains, obtain concentrated solution 2 after concentration and recovery ethanol to its no alcohol taste；
6) add ethanol in the concentrated solution 2 being obtained to described step 5, adjust its alcohol content to 90%, after stirring
Standing 48 hours, inclines and takes its supernatant to obtain supernatant 2；
7) take described step 5) supernatant 2 that obtains, carry out after concentration and recovery ethanol to its no alcohol taste receiving cream, China toad is obtained
Extract, and cold preservation.
Wherein, described step 4) in, the temperature during control precipitate with ethanol is 8 DEG C.
Wherein, described step 5) in, control vacuum in concentration process to be -0.07Mpa, control the temperature in concentration process
It is that 50 DEG C of gradients are incremented to final temperature for 60 DEG C by initial temperature.
Wherein, described step 6) in, the temperature during control precipitate with ethanol is 8 DEG C..
Wherein, described step 7) in, control the vacuum in concentration process to be -0.07Mpa, control the temperature in concentration process
Degree is that 50 DEG C of gradients are incremented to final temperature for 60 DEG C by initial temperature, controls the temperature of cold preservation to be -2 DEG C.
Embodiment 4
Take appropriate Cinobufacini extract prepared by embodiment 1,2 or 3, prepare injection, the piece of Cinobufacini extract
Agent, oral liquid, granule, powder, capsule, pill, soft capsule, ointment, nasal drop and suppository.
Although embodiment of the present invention is disclosed as above, it is not restricted to listed in description and embodiment
With.It can be applied to various suitable the field of the invention completely.For those skilled in the art, can be easily
Realize other modification.Therefore under the general concept being limited without departing substantially from claim and equivalency range, the present invention does not limit
In specific details.
Claims (7)
1. a kind of extraction process of Cinobufacini extract is it is characterised in that comprise the following steps：
1) Cutis Bufonis after taking 1 weight portion to clean, add the water of 3-10 parts by volume, use strainer filtering, obtain after decocting 30-60 minute
Filtrate 1 and filtering residue 1；
2) add the water of 2-6 parts by volume in described filtering residue 1, after decocting 20-40 minute, use strainer filtering, obtain filtrate 2 and filter
Slag 2；
3) by 2-in-1 to described filtrate 1 and filtrate and after be placed in concentration tank concentrate, obtain concentrated solution 1 after concentration；
4) add ethanol in described concentrated solution 1, the alcohol content adjusting concentrated solution, to 50-75%, stands 24-72 after stirring
Hour, incline and take its supernatant to obtain supernatant 1；
5) take described step 4) supernatant 1 that obtains, obtain concentrated solution 2 after concentration and recovery ethanol to its no alcohol taste；
6) add ethanol in the concentrated solution 2 being obtained to described step 5, adjust its alcohol content to 70-95%, quiet after stirring
Put 36-48 hour, incline and take its supernatant to obtain supernatant 2；
7) take described step 5) supernatant 2 that obtains, carry out after concentration and recovery ethanol to its no alcohol taste receiving cream, prepared cinobufacin carries
Take thing, and cold preservation.
2. the extraction process of Cinobufacini extract according to claim 1 is it is characterised in that described step 1) and step 2)
In filter screen filter pore size be 60 mesh or 80 mesh.
3. the extraction process of Cinobufacini extract according to claim 1 and 2 is it is characterised in that described step 3) in, control
Temperature in concentration process processed is 60 DEG C～85 DEG C, vacuum is -0.06Mpa～-0.09Mpa；Described step 4) in, control anti-
Temperature during answering is 0 DEG C～10 DEG C.
4. the extraction process of Cinobufacini extract according to claim 1 is it is characterised in that described step 5) in, control
Vacuum in concentration process be -0.06Mpa～-0.09Mpa, control concentration process in temperature by initial temperature be 40 DEG C～
50 DEG C of gradients are incremented to final temperature and are 55 DEG C～60 DEG C.
5. the extraction process of Cinobufacini extract according to claim 1 is it is characterised in that described step 6) in, control
Temperature in course of reaction is 0 DEG C～10 DEG C.
6. the extraction process of Cinobufacini extract according to claim 1 is it is characterised in that described step 7) in, control
Vacuum in concentration process be -0.06Mpa～-0.09Mpa, control concentration process in temperature by initial temperature be 40 DEG C～
50 DEG C of gradients are incremented to final temperature and are 55 DEG C～60 DEG C, control the temperature of cold preservation to be -2 DEG C～4 DEG C.
7. a kind of cinobufacin prepared by extraction process of the Cinobufacini extract as described in any one in claim 1-6 carries
Take thing in injection, tablet, oral liquid, granule, powder, capsule, pill, soft capsule, ointment, nasal drop and suppository
Application.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610848800.8A CN106432402A (en) | 2016-09-23 | 2016-09-23 | Extraction process of cinobufagin extract |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610848800.8A CN106432402A (en) | 2016-09-23 | 2016-09-23 | Extraction process of cinobufagin extract |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN106432402A true CN106432402A (en) | 2017-02-22 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201610848800.8A Pending CN106432402A (en) | 2016-09-23 | 2016-09-23 | Extraction process of cinobufagin extract |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114920795A (en) * | 2022-05-12 | 2022-08-19 | 赣江中药创新中心 | Preparation method of dried toad skin bufogenin lactone component |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1813802A (en) * | 2005-02-04 | 2006-08-09 | 安徽金蟾生化股份有限公司 | Bufonid skin extract production process |
-
2016
- 2016-09-23 CN CN201610848800.8A patent/CN106432402A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1813802A (en) * | 2005-02-04 | 2006-08-09 | 安徽金蟾生化股份有限公司 | Bufonid skin extract production process |
Non-Patent Citations (1)
| Title |
|---|
| 王晓东 等: "蟾皮提取分离方法及有效成分的研究进展", 《武警医学院学报》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114920795A (en) * | 2022-05-12 | 2022-08-19 | 赣江中药创新中心 | Preparation method of dried toad skin bufogenin lactone component |
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Application publication date: 20170222 |