CN106749470A - It is a kind of to extract the method that family's livestock bile prepares bile acid product - Google Patents
It is a kind of to extract the method that family's livestock bile prepares bile acid product Download PDFInfo
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- CN106749470A CN106749470A CN201611133949.4A CN201611133949A CN106749470A CN 106749470 A CN106749470 A CN 106749470A CN 201611133949 A CN201611133949 A CN 201611133949A CN 106749470 A CN106749470 A CN 106749470A
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- bile
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07J—STEROIDS
- C07J9/00—Normal steroids containing carbon, hydrogen, halogen or oxygen substituted in position 17 beta by a chain of more than two carbon atoms, e.g. cholane, cholestane, coprostane
- C07J9/005—Normal steroids containing carbon, hydrogen, halogen or oxygen substituted in position 17 beta by a chain of more than two carbon atoms, e.g. cholane, cholestane, coprostane containing a carboxylic function directly attached or attached by a chain containing only carbon atoms to the cyclopenta[a]hydrophenanthrene skeleton
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- Health & Medical Sciences (AREA)
- General Health & Medical Sciences (AREA)
- Medicines Containing Material From Animals Or Micro-Organisms (AREA)
- Medicines Containing Plant Substances (AREA)
Abstract
The method that family's livestock bile prepares bile acid product is extracted the invention discloses a kind of, step is as follows：Fresh domestic animal courage is taken, with 65% alcohol-pickled cleaning, domestic animal courage is shredded, family's livestock bile is taken out；Sodium hydroxide solution is added in taken bile, after standing, is adjusted with hydrochloric acid and is precipitated；Precipitation is collected by filtration, water and hydrogen peroxide solution is added, sodium carbonate solid powder is subsequently adding so that precipitation conversion, filtrate is collected by filtration, filtrate is adjusted with hydrochloric acid, after standing, filtering to be precipitated, and cleaned with water, and TBA crude product is can obtain after drying；Alcoholic solution is added in crude product, filtrate is collected by filtration, SDEB styrene diethylenebenzene extraction degreasing is added, takes alcohol layer and is adjusted with ammoniacal liquor, recovered alcohol solution, original volume is added water to, after adding calcium chloride water, by after wash-out and crystallization, vacuum drying treatment obtains final product bile acid fine work, whole preparation process mild condition of the present invention, reagent consumption is few, it is easy to be applied to industrialized production.
Description
Technical field
Engineering field is extracted the present invention relates to animal, it is specifically a kind of to extract the side that family's livestock bile prepares bile acid product
Method.
Background technology
Bile acid is the important component of bile, is played an important role in fat metabolism.Bile acid is primarily present in intestines liver
The circulatory system is simultaneously played a protective role by recycling.Only a small part bile acid enters peripheral circulation.Promote bile
The power of sour intestines liver circulation is the movement system of liver cell --- absorbs bile acid and is secreted into bile, cholecystokinin induction
Gallbladder contraction, small intestine propulsion wriggle, the active transport and blood of ileal mucosa are to pylic inflow.
At present, preparing bile acid mainly has chemical synthesis and the natural class of bile extraction method two.It is presently disclosed from natural
There is complex operation in the method that bile acid is extracted in bile, purity is relatively low, and yield is relatively low, and reagent consumption is big, relatively costly, difficult
The shortcomings of to be applied to industrialization；Chemical synthesis complex operation, methanol usage is big, with chloroform and methyl alcohol extracting cholesterol time-division
Layer is unintelligible, it is difficult to grasp, error easily occurs, is extremely difficult to separate the purpose of cholesterol and lipid, and cost is too high.
The content of the invention
The method that family's livestock bile prepares bile acid product is extracted it is an object of the invention to provide a kind of, to solve the above-mentioned back of the body
The problem proposed in scape technology.
To achieve the above object, the present invention provides following technical scheme：
A kind of to extract the method that family's livestock bile prepares bile acid product, processing step is as follows：
1）Fresh domestic animal courage is taken, with 65% alcohol-pickled 20~30min of cleaning, domestic animal courage is shredded, family's livestock bile is taken out；
2）1~3 times of sodium hydroxide solution of volume is added in taken bile, 30~50min of agitating heating, heating-up temperature is 50
~60 DEG C, be 2.2~4.6 with the salt acid for adjusting pH value that volumetric concentration is 30~35% when standing is cooled to 40 DEG C, after standing, is sunk
Conversion of forming sediment is complete；
3）Precipitation is collected by filtration, adds in 2~5 times of water of quality, add hydrogen peroxide solution to cause that concentration reaches mixing suspension
The 2.2~4.5% of volume, then add sodium carbonate solid powder by the 15~20% of bile quality so that precipitation conversion, filtering is received
Collection filtrate, it is 2.2~4.6 to adjust filtrate pH value with the hydrochloric acid that volumetric concentration is 30~35%, and after standing, filtering to precipitate, and use water
Cleaning is 6.5~7.5 to pH, and TBA crude product is can obtain after drying；
4）95% alcoholic solution is added in crude product, adjustment solution concentration to 50~60% stirs 30~50min, filtrate is collected by filtration,
By volume 1:1 adds styrene-divinylbenzene extraction degreasing, and it is 7.5~8.5 to take alcohol layer ammoniacal liquor regulation pH value, reclaims wine
Smart solution, adds water to original volume, and it is 12~15% calcium chloride waters to add mass volume ratio concentration, and 30~50min of stirring is to heavy
Form sediment complete, sediment is collected by filtration；
5）Sediment is washed with water to faint yellow, heating for dissolving, is filtered while hot, filtrate hydrochloric acid solution regulation pH value is 3~5,
Precipitation is collected by filtration, it is 6.5~7.5 that sediment is cleaned to pH with water, is eluted with 65% alcohol, and period is constantly examined with thin-layer chromatography
Survey, when outward appearance to be precipitated is single, collect eluent until finishing；
6）After adding mass ratio to be 1.2~1.5% activated carbon decolorizing in eluent, in recovered alcohol is evaporated under vacuum, obtain
Bile acid product crystallize, be placed in and 12h heated in 50~60 DEG C of water-baths, take out product crystallization -10~-5 DEG C be vacuum dried 3~
5h, obtains final product bile acid fine work.
As further scheme of the invention：The step 2）In time of repose be 1.5~3h.
As further scheme of the invention：The step 3）In time of repose be 3~5h.
As further scheme of the invention：The step 1）In sodium hydroxide solution mass volume ratio for 50~
90%。
Compared with prior art, the beneficial effects of the invention are as follows：Before preparation, alcohol-pickled cleaning is used, house is effectively ensured
Poultry courage quality；Health medicine is prepared using domestic animal bile extract, abundant raw material is cheap；Preparation method safety non-toxic, letter
It is single efficient, low cost；Whole preparation process mild condition, reagent consumption is few, it is easy to be applied to industrialized production.
Specific embodiment
The technical scheme in the embodiment of the present invention is clearly and completely described below, it is clear that described embodiment
Only a part of embodiment of the invention, rather than whole embodiments.Based on the embodiment in the present invention, the common skill in this area
The every other embodiment that art personnel are obtained under the premise of creative work is not made, belongs to the model of present invention protection
Enclose.
A kind of to extract the method that family's livestock bile prepares bile acid product in the embodiment of the present invention, one kind extracts family's livestock bile
The method for preparing bile acid product, processing step is as follows：
1）Fresh domestic animal courage is taken, with 65% alcohol-pickled 20~30min of cleaning, domestic animal courage is shredded, family's livestock bile is taken out；
2）1~3 times of sodium hydroxide solution of volume is added in taken bile, 30~50min of agitating heating, heating-up temperature is 50
~60 DEG C, wherein, the mass volume ratio of sodium hydroxide solution is 50~90%, is 30 with volumetric concentration when standing is cooled to 40 DEG C
~35% salt acid for adjusting pH value is 2.2~4.6, stands 1.5~3h, and precipitation conversion is complete；
3）Precipitation is collected by filtration, adds in 2~5 times of water of quality, add hydrogen peroxide solution to cause that concentration reaches mixing suspension
The 2.2~4.5% of volume, then add sodium carbonate solid powder by the 15~20% of bile quality so that precipitation conversion, filtering is received
Collection filtrate, it is 2.2~4.6 to adjust filtrate pH value with the hydrochloric acid that volumetric concentration is 30~35%, stands 3~5h, and filtering to precipitate,
It is 6.5~7.5 to be cleaned with water to pH, and TBA crude product is can obtain after drying；
4）95% alcoholic solution is added in crude product, adjustment solution concentration to 50~60% stirs 30~50min, filtrate is collected by filtration,
By volume 1:1 adds styrene-divinylbenzene extraction degreasing, and it is 7.5~8.5 to take alcohol layer ammoniacal liquor regulation pH value, reclaims wine
Smart solution, adds water to original volume, and it is 12~15% calcium chloride waters to add mass volume ratio concentration, and 30~50min of stirring is to heavy
Form sediment complete, sediment is collected by filtration；
5）Sediment is washed with water to faint yellow, heating for dissolving, is filtered while hot, filtrate hydrochloric acid solution regulation pH value is 3~5,
Precipitation is collected by filtration, it is 6.5~7.5 that sediment is cleaned to pH with water, is eluted with 65% alcohol, and period is constantly examined with thin-layer chromatography
Survey, when outward appearance to be precipitated is single, collect eluent until finishing；
6）After adding mass ratio to be 1.2~1.5% activated carbon decolorizing in eluent, in recovered alcohol is evaporated under vacuum, obtain
Bile acid product crystallize, be placed in and 12h heated in 50~60 DEG C of water-baths, take out product crystallization -10~-5 DEG C be vacuum dried 3~
5h, obtains final product bile acid fine work.
Health medicine is prepared using domestic animal bile extract, abundant raw material is cheap；Preparation method safety non-toxic, simply
Efficiently, low cost；Whole preparation process mild condition, reagent consumption is few, it is easy to be applied to industrialized production.
It is obvious to a person skilled in the art that the invention is not restricted to the details of above-mentioned one exemplary embodiment, Er Qie
In the case of without departing substantially from spirit or essential attributes of the invention, the present invention can be in other specific forms realized.Therefore, no matter
From the point of view of which point, embodiment all should be regarded as exemplary, and be nonrestrictive, the scope of the present invention is by appended power
Profit requires to be limited rather than described above, it is intended that all in the implication and scope of the equivalency of claim by falling
Change is included in the present invention.Any reference in claim should not be considered as the claim involved by limitation.
Claims (4)
1. it is a kind of to extract the method that family's livestock bile prepares bile acid product, it is characterised in that processing step is as follows：
1）Fresh domestic animal courage is taken, with 65% alcohol-pickled 20~30min of cleaning, domestic animal courage is shredded, family's livestock bile is taken out；
2）1~3 times of sodium hydroxide solution of volume is added in taken bile, 30~50min of agitating heating, heating-up temperature is 50
~60 DEG C, be 2.2~4.6 with the salt acid for adjusting pH value that volumetric concentration is 30~35% when standing is cooled to 40 DEG C, after standing, is sunk
Conversion of forming sediment is complete；
3）Precipitation is collected by filtration, adds in 2~5 times of water of quality, add hydrogen peroxide solution to cause that concentration reaches mixing suspension
The 2.2~4.5% of volume, then add sodium carbonate solid powder by the 15~20% of bile quality so that precipitation conversion, filtering is received
Collection filtrate, it is 2.2~4.6 to adjust filtrate pH value with the hydrochloric acid that volumetric concentration is 30~35%, and after standing, filtering to precipitate, and use water
Cleaning is 6.5~7.5 to pH, and TBA crude product is can obtain after drying；
4）95% alcoholic solution is added in crude product, adjustment solution concentration to 50~60% stirs 30~50min, filtrate is collected by filtration,
By volume 1:1 adds styrene-divinylbenzene extraction degreasing, and it is 7.5~8.5 to take alcohol layer ammoniacal liquor regulation pH value, reclaims wine
Smart solution, adds water to original volume, and it is 12~15% calcium chloride waters to add mass volume ratio concentration, and 30~50min of stirring is to heavy
Form sediment complete, sediment is collected by filtration；
5）Sediment is washed with water to faint yellow, heating for dissolving, is filtered while hot, filtrate hydrochloric acid solution regulation pH value is 3~5,
Precipitation is collected by filtration, it is 6.5~7.5 that sediment is cleaned to pH with water, is eluted with 65% alcohol, and period is constantly examined with thin-layer chromatography
Survey, when outward appearance to be precipitated is single, collect eluent until finishing；
6）After adding mass ratio to be 1.2~1.5% activated carbon decolorizing in eluent, in recovered alcohol is evaporated under vacuum, obtain
Bile acid product crystallize, be placed in and 12h heated in 50~60 DEG C of water-baths, take out product crystallization -10~-5 DEG C be vacuum dried 3~
5h, obtains final product bile acid fine work.
2. the method that a kind of extraction man livestock bile according to claim 1 prepares bile acid product, it is characterised in that described
Step 2）In time of repose be 1.5~3h.
3. the method that a kind of extraction man livestock bile according to claim 1 prepares bile acid product, it is characterised in that described
Step 3）In time of repose be 3~5h.
4. the method that a kind of extraction man livestock bile according to claim 1 prepares bile acid product, it is characterised in that described
Step 1）In sodium hydroxide solution mass volume ratio be 50~90%.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611133949.4A CN106749470A (en) | 2016-12-10 | 2016-12-10 | It is a kind of to extract the method that family's livestock bile prepares bile acid product |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611133949.4A CN106749470A (en) | 2016-12-10 | 2016-12-10 | It is a kind of to extract the method that family's livestock bile prepares bile acid product |
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| Publication Number | Publication Date |
|---|---|
| CN106749470A true CN106749470A (en) | 2017-05-31 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201611133949.4A Pending CN106749470A (en) | 2016-12-10 | 2016-12-10 | It is a kind of to extract the method that family's livestock bile prepares bile acid product |
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1528779A (en) * | 2003-09-29 | 2004-09-15 | 华东理工大学 | Method for preparing cheodexycholic acid |
| CN1775798A (en) * | 2005-12-13 | 2006-05-24 | 山东博尔德生物科技有限公司 | Method for producing high-purity chenodeoxy cholic acid from poultry and livestock bile |
-
2016
- 2016-12-10 CN CN201611133949.4A patent/CN106749470A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1528779A (en) * | 2003-09-29 | 2004-09-15 | 华东理工大学 | Method for preparing cheodexycholic acid |
| CN1775798A (en) * | 2005-12-13 | 2006-05-24 | 山东博尔德生物科技有限公司 | Method for producing high-purity chenodeoxy cholic acid from poultry and livestock bile |
Non-Patent Citations (1)
| Title |
|---|
| 李冠霖: "郎德鹅胆汁提取纯化鹅去氧胆酸工艺技术研究", 《广西大学农业推广硕士学位论文》 * |
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Application publication date: 20170531 |