CN105884847A - Chenodeoxycholic acid extraction method - Google Patents
Chenodeoxycholic acid extraction method Download PDFInfo
- Publication number
- CN105884847A CN105884847A CN201410495532.7A CN201410495532A CN105884847A CN 105884847 A CN105884847 A CN 105884847A CN 201410495532 A CN201410495532 A CN 201410495532A CN 105884847 A CN105884847 A CN 105884847A
- Authority
- CN
- China
- Prior art keywords
- carrying
- acid
- value
- precipitates
- volume ratio
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Landscapes
- Steroid Compounds (AREA)
Abstract
The invention discloses a chenodeoxycholic acid extraction method. The method comprises A, adding a sodium hydroxide solution into bile according to a volume ratio of 3-6: 1, carrying out uniform heating and adjusting pH to 1.2-5.5 through hydrochloric acid with a volume concentration of 20-40% so that precipitates are produced, B, filtering the precipitates to obtain black green paste, adding a sodium chloride solution into the paste according to a mass ratio of 2-3: 1, heating the mixed solution, carrying out water washing until pH of 6.8-7.5 and carrying out drying to obtain a total bile acid crude product, C, dissolving the crude product through methanol with a concentration of 95% along with stirring, filtering to remove insoluble substances, adding n-hexane into the solution according to a ratio of 1: 1, carrying out extraction degreasing, adding a barium chloride aqueous solution with a mass-volume ratio concentration of 10% into the solution until complete precipitation and carrying out filtration to obtain precipitates, D, washing the precipitates by water until a yellowy color, carrying out dissolution, carrying out filtration, adjusting pH of the filtrate to 3-7 through hydrochloric acid, separating the precipitates, washing the precipitates through water until pH of 7.5, carrying out drying for 2-7h and carrying out decoloring through chlorine dioxide and polyaluminum chloride to obtain a chenodeoxycholic acid product. The method realizes waste use and reduces a cost.
Description
Technical field
The present invention relates to bioengineering field, it is more particularly related to one extracts chenodeoxycholic acid from goose Fel Anas domestica juice
Method.
Background technology
Cholic acid is a kind of sterin, is the one that in four kinds of primary bile acid of the mankind, content is the abundantest, glycocholic acid derivative from it and
Taurocholic acid is the primary bile acid of the mankind.The bile salts (sodium salt of bile acid) that liver is secreted in bile is strong emulsifying agent.
After bile flows through upper part of small intestine, bile salts chyle fat, helps its digested absorption.Fatty acid and glycerol at chyle fat droplet
Ester is by after small intestinal lower absorbent, and bile salts is also heavily absorbed.They return to liver and are reused, and therefore, bile salts always exists
Circulate between liver and small intestinal.Bile salts is not only to fat, also to all fat-soluble nutritious compound absorption particular importances.When because suffering from some
When the generation of disease generation bile salts or hyposecretion, will occur not digesting and unabsorbed fat in feces.Now, liposoluble
Property vitamin A. D. E, K can not fully absorb, and make people cause the trophism of vitamin A to lack.
Clinical conventional animal cholic acid has ursodesoxycholic acid, chenodeoxycholic acid and Hyodeoxycholic Acid.Wherein ursodesoxycholic acid is Bears
The special composition of gallbladder, owing to Bears is protection animal, so Fel Ursi resource is nervous, cost is high.And chenodeoxycholic acid is ursodeoxycholic
The isomer of acid, has stronger choleretic effect equally.
Application No. 03151475.8 Chinese invention patent application file discloses " preparation method of a kind of chenodeoxycholic acid ", should
Method provides a kind of industrialized process for preparing of extraction purification chenodeoxycholic acid from poultry and animal bile, and its process includes leading to
Cross alkali liquor saponification bile, the preparation calcium precipitation of TOTAL BILE ACID TBA, hydrogen peroxide and decolorizing with activated carbon, sodium carbonate and hydrochloric acid and convert goose
The steps such as oxycholic acid calcium precipitation and purification with macroreticular resin.The method uses calcium salt precipitation method, and settling velocity is slow, and efficiency is low,
And hydrogen peroxide and activated carbon decolorizing effect the most undesirable.
Summary of the invention
Low in order to solve deposition efficiency mentioned above, that decolorizing effect is bad problem, the present invention provides one to utilize factory to discard
The poultry bile of thing extracts the method for chenodeoxycholic acid, can be salvaged, and reduces cost, expands medicine resource.
In order to realize above-mentioned technical purpose, technical scheme is as follows:
A kind of extracting method of chenodeoxycholic acid, it is characterised in that: processing step is as follows:
A, adding 3～6 times of volume sodium hydroxide solutions in taken bile, stir evenly and be heated to 80～90 DEG C, insulation is 1～2 little
It is cooled to 50～70 DEG C time after, adjusts pH value to be 1.2～5.5 with the hydrochloric acid of volumetric concentration 20～40%, stand 3～5 hours,
Produce precipitation；
B, filtering to obtain blackish green paste, the sodium chloride solution adding 2～3 times of quality heats 5～8 hours, stands, filters
Precipitation, washing with water to pH value is 6.8～7.5, is dried, obtains TOTAL BILE ACID TBA crude product at-10 DEG C～1 DEG C；
C, crude product add 95% methanol stirring and dissolving, filter insoluble matter, add n-hexane extraction defat by 1: 1, take methanol layer and use
Ammonia adjusts pH value to be 8～10, reclaims methanol, adds water to original volume, adds the barium chloride that mass volume ratio concentration is 10% water-soluble
Liquid is complete to precipitation, leaching precipitate；
D, precipitate is washed with water to color yellowish, heating for dissolving, filtered while hot, filtrate hydrochloric acid adjust pH value be 3～7, separate out
Precipitation, precipitate washes with water to pH value=7.5, and-12 DEG C～2 DEG C are dried 2～7 hours, then with chlorine dioxide and aluminium polychlorid
Decolour to obtain CDCA acid product.
The mass volume ratio concentration of sodium hydroxide solution described in step is 48～92%.
The mass volume ratio concentration of sodium chloride solution described in stepb is 58～82%.
Crude product and the mass volume ratio of 95% methanol described in step C are 1: 2.1～8.1.
The mass ratio between chlorine dioxide and aluminium polychlorid described in step D is 1: 1.1～2.6, and gross weight is precipitation
2～5 times of thing.
The beneficial effects of the present invention is: the invention provides a kind of method extracting chenodeoxycholic acid from goose Fel Anas domestica juice, utilize
The poultry bile of plant wastes extracts the method for chenodeoxycholic acid, can be salvaged, and reduces cost, expands medicine resource.1、
The present invention uses goose bile to extract chenodeoxycholic acid, abundant raw material and cheap, and effect is similar with ursodesoxycholic acid；2, use
Sodium hydroxide pellets, settling rate faster, improves the efficiency of production, substantially increases production capacity, reduce cost；3, this
Chenodeoxycholic acid is decoloured by bright employing chlorine dioxide and aluminium polychlorid cooperation, and decolorizing effect is more preferable.
Detailed description of the invention
Embodiment one
A, in taken bile add 2 times of volumes, mass volume ratio concentration be the sodium hydroxide solution of 50%, stir evenly and be heated to
80 DEG C, after being incubated 1 hour, it is cooled to 50 DEG C, adjusts pH value to be 1.2 with the hydrochloric acid of volumetric concentration 20%, stand 3 hours, produce
Raw precipitation；
B, filter to obtain blackish green paste, add 1 times of quality, mass volume ratio concentration be 60% sodium chloride solution heating 5
Hour, stand, filter to obtain precipitation, washing with water to pH value is to be dried at 6.8 ,-10 DEG C, obtains TOTAL BILE ACID TBA crude product；
C, crude product add 95% methanol stirring and dissolving, filter insoluble matter, and the mass volume ratio of crude product and 95% methanol is 1: 2, presses
Add n-hexane extraction defat at 1: 1, takes methanol layer ammonia and adjusts pH value to be 8.5, reclaims methanol, add water to original volume, add
Mass volume ratio concentration be 10% barium chloride solution to precipitation completely, leaching precipitate；
D, precipitate is washed with water to color yellowish, heating for dissolving, filtered while hot, filtrate hydrochloric acid adjust pH value be 2.5, separate out
Precipitation, precipitate washes with water to pH value=7.5, and-12 DEG C are dried 2 hours, then decolour with chlorine dioxide and aluminium polychlorid
CDCA acid product, the mass ratio between chlorine dioxide and aluminium polychlorid is 1: 1, and gross weight is sedimentary 2 times.
Embodiment two
A, in taken bile add 5 times of volumes, mass volume ratio concentration be the sodium hydroxide solution of 90%, stir evenly and be heated to
90 DEG C, after being incubated 2 hours, it is cooled to 70 DEG C, adjusts pH value to be 5.5 with the hydrochloric acid of volumetric concentration 40%, stand 5 hours, produce
Raw precipitation；
B, filter to obtain blackish green paste, add 2 times of quality, mass volume ratio concentration be 80% sodium chloride solution heating 8
Hour, stand, filter to obtain precipitation, washing with water to pH value is to be dried at 7.5,1 DEG C, obtains TOTAL BILE ACID TBA crude product；
C, crude product add 95% methanol stirring and dissolving, filter insoluble matter, and the mass volume ratio of crude product and 95% methanol is 1: 8, presses
Add n-hexane extraction defat at 1: 1, takes methanol layer ammonia and adjusts pH value to be 8.5～10, reclaims methanol, add water to original volume,
Add the barium chloride solution that mass volume ratio concentration is 10% complete to precipitation, leaching precipitate；
D, precipitate is washed with water to color yellowish, heating for dissolving, filtered while hot, filtrate hydrochloric acid adjust pH value be 6.5, separate out
Precipitation, precipitate washes with water to pH value=7.5,2 DEG C be dried 7 hours, then with chlorine dioxide and aluminium polychlorid decolour goose goes
Oxycholic acid product, the mass ratio between chlorine dioxide and aluminium polychlorid is 1: 2.5, and gross weight is sedimentary 5 times.
Embodiment three
A, in taken bile add 3.5 times of volumes, mass volume ratio concentration be the sodium hydroxide solution of 70%, stir evenly heating
To 85 DEG C, after being incubated 1.5 hours, it is cooled to 60 DEG C, adjusts pH value to be 3.2 with the hydrochloric acid of volumetric concentration 30%, stand 4 hours,
Produce precipitation；
B, filter to obtain blackish green paste, add 1.5 times of quality, mass volume ratio concentration be 70% sodium chloride solution heating 6.5
Hour, stand, filter to obtain precipitation, washing with water to pH value is to be dried at 7.2 ,-5 DEG C, obtains TOTAL BILE ACID TBA crude product；
C, crude product add 95% methanol stirring and dissolving, filter insoluble matter, and the mass volume ratio of crude product and 95% methanol is 1: 5, presses
Add n-hexane extraction defat at 1: 1, takes methanol layer ammonia and adjusts pH value to be 9, reclaims methanol, add water to original volume, add matter
Measure the barium chloride solution that volume by volume concentration is 10% complete to precipitation, leaching precipitate；
D, washing precipitate to color with water yellowish, heating for dissolving, filtered while hot, filtrate hydrochloric acid adjusts pH value to be 5, and it is heavy to separate out
Forming sediment, precipitate washes with water to pH value=7.5, and-6 DEG C are dried 2～7 hours, then decolour to obtain goose with chlorine dioxide and aluminium polychlorid
Deoxycholic acid product, the mass ratio between chlorine dioxide and aluminium polychlorid is 1: 1.5, and gross weight is sedimentary 3.5 times.
Embodiment four
A, in taken bile add 4 times of volumes, mass volume ratio concentration be the sodium hydroxide solution of 85%, stir evenly and be heated to
88 DEG C, after being incubated 1.5 hours, it is cooled to 65 DEG C, adjusts pH value to be 5 with the hydrochloric acid of volumetric concentration 35%, stand 4.5 hours,
Produce precipitation；
B, filter to obtain blackish green paste, add 1.5 times of quality, mass volume ratio concentration be 75% sodium chloride solution heating 7.5
Hour, stand, filter to obtain precipitation, washing with water to pH value is to be dried at 7,0 DEG C, obtains TOTAL BILE ACID TBA crude product；
C, crude product add 95% methanol stirring and dissolving, filter insoluble matter, and the mass volume ratio of crude product and 95% methanol is 1: 7, presses
Add n-hexane extraction defat at 1: 1, takes methanol layer ammonia and adjusts pH value to be 9.5, reclaims methanol, add water to original volume, add
Mass volume ratio concentration be 10% barium chloride solution to precipitation completely, leaching precipitate；
D, precipitate is washed with water to color yellowish, heating for dissolving, filtered while hot, filtrate hydrochloric acid adjust pH value be 5.5, separate out
Precipitation, precipitate washes with water to pH value=7.5, and-10 DEG C are dried 3 hours, then decolour to obtain goose with chlorine dioxide and aluminium polychlorid
Deoxycholic acid product, the mass ratio between chlorine dioxide and aluminium polychlorid is 1: 2.5, and gross weight is sedimentary 4.5 times.
Claims (5)
1. the extracting method of a chenodeoxycholic acid, it is characterised in that: processing step is as follows: A, in taken bile add 3～
6 times of volume sodium hydroxide solutions, stir evenly and are heated to 80～90 DEG C, be cooled to 50～70 DEG C, use volume after being incubated 1～2 hour
Concentration 20～40% hydrochloric acid adjust pH value to be 1.2～5.5, stands 3～5 hours, produces and precipitate；B, filter to obtain blackish green cream
Shape thing, the sodium chloride solution adding 2～3 times of quality heats 5～8 hours, stands, and filters and to obtain precipitation, washes with water to pH value and is
6.8～7.5, it is dried at-10 DEG C～1 DEG C, obtains TOTAL BILE ACID TBA crude product；C, crude product add 95% methanol stirring and dissolving, filter insoluble
Thing, adds n-hexane extraction defat by 1: 1, takes methanol layer ammonia and adjusts pH value to be 8～10, reclaims methanol, add water to former
Volume, adds the barium chloride solution that mass volume ratio concentration is 10% and extremely precipitates completely, leaching precipitate；D, by precipitate
Washing with water to color yellowish, heating for dissolving, filtered while hot, filtrate hydrochloric acid is adjusted pH value to be 3～7, is separated out precipitation, precipitate use
Being washed to pH value=7.5 ,-12 DEG C～2 DEG C are dried 2～7 hours, then decolour to obtain CDCA with chlorine dioxide and aluminium polychlorid
Acid product.
The extracting method of a kind of chenodeoxycholic acid the most according to claim 1, it is characterised in that: described in step
The mass volume ratio concentration of sodium hydroxide solution is 48～92%.
The extracting method of a kind of chenodeoxycholic acid the most according to claim 1, it is characterised in that: described in stepb
The mass volume ratio concentration of sodium chloride solution is 58～82%.
The extracting method of a kind of chenodeoxycholic acid the most according to claim 1, it is characterised in that: described in step C
The mass volume ratio of crude product and 95% methanol is 1: 2.1～8.1.
The extracting method of a kind of chenodeoxycholic acid the most according to claim 1, it is characterised in that: described in step D
Mass ratio between chlorine dioxide and aluminium polychlorid is 1: 1.1～2.6, and gross weight is sedimentary 2～5 times.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410495532.7A CN105884847A (en) | 2014-09-17 | 2014-09-17 | Chenodeoxycholic acid extraction method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410495532.7A CN105884847A (en) | 2014-09-17 | 2014-09-17 | Chenodeoxycholic acid extraction method |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN105884847A true CN105884847A (en) | 2016-08-24 |
Family
ID=57000156
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201410495532.7A Pending CN105884847A (en) | 2014-09-17 | 2014-09-17 | Chenodeoxycholic acid extraction method |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN105884847A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106883281A (en) * | 2017-03-08 | 2017-06-23 | 眉山市新功生物科技有限公司 | The method that chenodeoxycholic acid is extracted from duck bile |
-
2014
- 2014-09-17 CN CN201410495532.7A patent/CN105884847A/en active Pending
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106883281A (en) * | 2017-03-08 | 2017-06-23 | 眉山市新功生物科技有限公司 | The method that chenodeoxycholic acid is extracted from duck bile |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN110294784B (en) | Method for extracting oryzanol by taking rice bran oil refined soapstock as raw material | |
| CN100556914C (en) | A kind of method that from Fel Sus domestica, prepares the high purity Hyodeoxycholic Acid | |
| CN104004592B (en) | A kind of method simultaneously extracting essential oil and pectin from fresh peel of Citrus reticulata Blanco | |
| CN102757515B (en) | Method for extracting high-purity flavonoid and pectin from citrus peel | |
| CN104130333A (en) | Method for synchronous production of anthocyanidin, starch, cellulose and protein by using purple sweet potato | |
| CN103059095A (en) | Green extraction technology for comprehensive and efficient utilization of Dioscorea zingiberensis resource | |
| CN110305179B (en) | Method for extracting oryzanol by taking unsaponifiable matters refined from rice bran oil as raw materials | |
| CN102977226A (en) | Method for preparing pectin from shaddock peels | |
| CN107057829A (en) | The technique of separating-purifying arhat fruit seed oil in a kind of extraction slag from Momordica grosvenori | |
| CN102453069A (en) | Method for extracting chenodeoxycholic acid from goose and duck bile | |
| CN103483403B (en) | A kind of circulation extracting method of hesperidine of purifying from tangerine slag | |
| CN102630890B (en) | Method for preparing leechee or longan pulp powder | |
| CN105884847A (en) | Chenodeoxycholic acid extraction method | |
| CN106146686A (en) | A kind of technique utilizing Receptaculum Helianthi industrialized production pectin | |
| CN107286071B (en) | A method of extracting bilirubin and cholic acid co-production cholesterol, lecithin from bile | |
| CN104829746A (en) | Method for extracting pectin from citrus peel and keeping aroma in pectin | |
| CN105481927B (en) | A method of extracting duck cholic acid and chenodeoxycholic acid from duck bile | |
| CN104341538A (en) | A separation and preparing method of high-HG-content sunflower pectin | |
| CN103992300B (en) | A kind of method extracting pycnogenols from tartary buckwheat bran | |
| CN105272989A (en) | Method for preparing chlorophyll sodium copper from mulberry leaves | |
| EP3858848B1 (en) | Method for preparing oryzanol by using soapstock containing oryzanol as raw material | |
| CN105884848A (en) | Hyodeoxycholic acid extraction method | |
| CN102285949B (en) | Method for extracting chrysin from passiflora edulis fruit residue obtained after juicing | |
| CN105481928B (en) | A kind of method that lithocholic acid is removed from chenodeoxycholic acid | |
| CN106277516B (en) | The method of water reuse is adsorbed in a kind of production of stevioside |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20160824 |
|
| WD01 | Invention patent application deemed withdrawn after publication |