CN102485740A - Technology for extracting chenodeoxycholic acid from poultry bile - Google Patents
Technology for extracting chenodeoxycholic acid from poultry bile Download PDFInfo
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- CN102485740A CN102485740A CN2010105778478A CN201010577847A CN102485740A CN 102485740 A CN102485740 A CN 102485740A CN 2010105778478 A CN2010105778478 A CN 2010105778478A CN 201010577847 A CN201010577847 A CN 201010577847A CN 102485740 A CN102485740 A CN 102485740A
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- chenodiol
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Abstract
The invention relates to a technology for extracting chenodeoxycholic acid from poultry bile. The technology comprises: adding poultry bile into caustic soda, and boiling the mixture for hydrolysis, adding a swelling solvent composed of an organic solvent and carbon dioxide into a hydrolysis liquid, conducting pressurized stirring and esterification, and extracting a chenodeoxycholic acid crude product from poultry bile, adding a calcium salt to for precipitation, thus obtaining cholate, washing the precipitate with purified water and adjusting the pH with hydrochloric acid so as to separate out a chenodeoxycholic acid precipitate, carrying out pressurized extraction with a swelling solvent composed of an organic solvent and carbon dioxide, reducing the pressure to separate out a chenodeoxycholic acid finished product. The technology of the invention has the characteristics of simple process, less organic solvent consumption, as well as high yield and purity product.
Description
Technical field
A kind of technology of from poultry bile, extracting Chenodiol belongs to the extraction process that relates to effective constituent in the animal viscera.
Background technology
Chenodiol is to have the medicine of correcting saturated cholelith and dissolving cholelith.The method of current extraction Chenodiol is a lot.For example: CN031514758 propose a kind of with poultry bile through saponification, calcium precipitation, ydrogen peroxide 50 and activated carbon decolorizing, yellow soda ash and hydrochloric acid transform Chenodiol deposition, the production Chenodiol method of purification with macroreticular resin; CN200510045346 proposes to prepare Chenodiol with poultry bile through saponification, neutralization, chromatography column chromatography and ultrafiltration; CN200610046652 proposes to prepare Chenodiol with Fel Gallus domesticus through heating, saponification, the decolouring of ethanol zeyssatite, gasoline degreasing, barium oxide precipitate and separate; CN1432579 provides a kind of exquisite method of Chenodiol bullion, and the Chenodiol bullion is used acetic acid ethyl dissolution, with the method for weak ammonia extracting impurities.But said extracted technology is more numerous and diverse, productive rate is low, purity is not high.For this reason, it is simple to seek a kind of extraction Chenodiol technology, increases productive rate and purity, raises the efficiency, and reduces the method for polluting and is still the content that presses for research.
Summary of the invention
The purpose of this invention is to provide a kind of from poultry bile, to extract the technology of Chenodiol; The present invention be directed to the poultry bile is raw material; Through technological processs such as hydrolysis, esterification, extraction, purifying, the extraction process that the expanded solvents system combines with esterification process, the function that enlarges with the chemical property differentiation of other compositions after utilizing Chenodiol by esterification; And improve dissolving power, the method for separation and purification Chenodiol with the pressure of less solvent through the raising system.
What is called expanded solvents system is meant in a small amount of organic solvent and is adding high-pressure carbon dioxide; High-pressure carbon dioxide and organic solvent dissolve each other; Impel the sharply formed liquid of expansion of its volume, this liquid has the density of quasi-liquid, seemingly the characteristics of the good solvent intensity of diffustivity and organic solvent as the gas; Particularly solubility with pressure changes with exponential form enhancing under coldcondition; And liquid polarity is adjustable, and solvent load significantly reduces, and chemical reaction process, transformation efficiency and selectivity are all strengthened greatly.
The scheme of technical solution problem of the present invention is:
1, poultry bile is added caustic soda and boil hydrolysis in the certain temperature condition;
2, hydrolyzed solution is neutralized to neutrality with hydrochloric acid;
3, the hydrolyzed solution after the neutralization joins the expanded solvents of being made up of polar organic solvent and carbonic acid gas, and pressurization is stirred under normal temperature condition, and esterification also extracts the Chenodiol bullion in the poultry bile;
4, above-mentioned solution reduces and adds calcium salt behind pressure to the normal pressure and separate out deposition, abandon after the filtration filtrate total cholic acid salt;
5, total cholic acid salt is added the pure water washing, regulate pH value with hydrochloric acid behind the collection aqueous solution, separate out the Chenodiol deposition, it is dry to be neutralized to neutral final vacuum with weak ammonia behind the precipitation separation;
6, dried Chenodiol bullion is formed and pressurization with organic solvent and carbonic acid gas, the normal temperature condition extraction.Chenodiol is separated out in step-down then, and vacuum-drying is finished product.
Embodiment
Specify the present invention below in conjunction with embodiment:
Embodiment 1:
(1) the 100kg poultry bile is added 10kg-20kg sodium hydroxide and stir, heated and boiled 15h-22h processes hydrolyzed solution;
(2) be neutralized to PH7 with hydrochloric acid;
(3) hydrolyzed solution after the neutralization joins in the expanded solvents of being made up of 10%-20% methyl alcohol and 80%-90% carbonic acid gas, and pressurization 4MPa-15MPa, normal temperature condition be maintenance 0.5h-5.0h down, is depressurized to 0.1MPa then, and Chenodiol is by esterification and extract;
(4) above-mentioned solution reduces pressure to normal pressure, adds 8kg-12kg calcium chloride, separates out deposition; Separate with rotating speed 3500r/min-7000r/min with separating machine; Discard filtrating, with Vacuumdrier at vacuum tightness 0.01Mpa-0.05Mpa, 50 ℃-80 ℃ of temperature; Time 0.5h-1.0h is dry, gets total cholic acid salt;
(5) above-mentioned total cholic acid salt is added 1 times of-2 times of pure water washing 2 times-5 times; Regulate PH3-PH5 with hydrochloric acid after collecting the aqueous solution; Separate out the Chenodiol deposition; With separating machine with rotating speed 3500r/min-7000r/min precipitation separation, after the deposition after the separation is neutralized to neutrality with 3mol/L-5mol/L ammoniacal liquor, with Vacuumdrier at vacuum tightness 0.01MPa-0.5MPa, 60 ℃-80 ℃ of temperature, oven dry 1h-6h;
(6) dried bullion is with the expanded solvents pressurization 2MPa-15MPa of non-polar organic solvent 2%-20% chloroform and 80%-98% carbonic acid gas composition; Extraction 0.5h-2.0h is depressurized to 0.1MPa-1.5MPa again and separates out Chenodiol under the normal temperature condition; With vacuum tightness 0.01MPa-0.1MPa, 50 ℃ of-80 ℃ of dryings of temperature are product with Vacuumdrier.
Embodiment 2:
(1) the 100kg poultry bile is added 8kg-20kg sodium hydroxide and stir, heat 90 ℃-110 ℃ and boil 15h-24h;
(2) reduce to normal temperature and be neutralized to PH7 with 3mol/L-18mol/L sulfuric acid;
(3) above-mentioned solution adding 10kg-20kg calcium chloride is separated out deposition, and the flame filter press filtration with the 10um-30um filter cloth gets total cholic acid salt;
(4) total cholic acid salt is added 1 times of-3 times of pure water washing; Regulate PH3 with 3mol/L-18mol/L sulfuric acid after collecting the aqueous solution; Separate out the Chenodiol deposition; After being neutralized to neutrality with the 0.1mol/L-1.0mol/L dilute sodium carbonate behind the precipitation separation, be 0.01MPa-0.1MPa in vacuum tightness, 60 ℃ of-80 ℃ of dry 0.5h-5h of temperature:
(5) dried Chenodiol bullion is with the pressurization 3.0MPa-10.0MPa of expanded solvents system of 5%-20% chloroform and 5%-10% ethanol and 500L-1000L carbonic acid gas composition; Normal temperature condition is extraction 0.5h-2.0h down; Be depressurized to 1.5MPa-2.5MPa then, separate out Chenodiol.
Claims (3)
1. technology of from poultry bile, extracting Chenodiol is characterized in:
(1), poultry bile is added caustic soda and boil hydrolysis in the certain temperature condition;
(2), hydrolyzed solution is neutralized to neutrality with hydrochloric acid;
(3), the hydrolyzed solution after the neutralization joins the expanded solvents of being made up of polar organic solvent and carbonic acid gas, the stirring of under normal temperature condition, pressurizeing extracts the Chenodiol bullion in the poultry bile;
(4), above-mentioned solution reduces and to add calcium salt behind pressure to the normal pressure and separate out deposition, abandon after the filtration filtrate cholate;
(5), total cholic acid salt is added the pure water washing, regulate pH value with hydrochloric acid after collecting the aqueous solution, separate out the Chenodiol deposition, it is dry to be neutralized to neutral final vacuum with weak ammonia behind the precipitation separation;
(6), dried Chenodiol bullion forms and pressurization with organic solvent and carbonic acid gas, the normal temperature condition extraction, Chenodiol is separated out in step-down then, vacuum-drying is finished product.
2. a kind of technology of from poultry bile, extracting Chenodiol as claimed in claim 1; The composition that it is characterized in that expanded solvents both can be made up of polar organic solvent 10%-20% methyl alcohol and 80%-90% carbonic acid gas, also can be that non-polar solvent 2.0%-20% chloroform and 80%-98% carbonic acid gas are formed.
3. a kind of Chenodiol technology of from poultry bile, extracting as claimed in claim 1 is characterized in that the expanded solvents applied pressure is 2MPa-15MPa, and separating pressure is 0.1MPa-1.5MPa.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2010105778478A CN102485740A (en) | 2010-12-01 | 2010-12-01 | Technology for extracting chenodeoxycholic acid from poultry bile |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2010105778478A CN102485740A (en) | 2010-12-01 | 2010-12-01 | Technology for extracting chenodeoxycholic acid from poultry bile |
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| CN102485740A true CN102485740A (en) | 2012-06-06 |
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| CN2010105778478A Pending CN102485740A (en) | 2010-12-01 | 2010-12-01 | Technology for extracting chenodeoxycholic acid from poultry bile |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103214538A (en) * | 2013-04-28 | 2013-07-24 | 广西北斗星动物保健品有限公司 | Method for separation and purification of bound total bile acid in bile paste |
| CN105418715A (en) * | 2015-12-28 | 2016-03-23 | 成都市新功生物科技有限公司 | Method for extracting chenodeoxycholic acid by carbon dioxide supercritical extraction method |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1850846A (en) * | 2006-05-23 | 2006-10-25 | 辽宁百隆生物工程有限公司 | Production method for extracting chenodeoxycholic acid using chicken gall |
-
2010
- 2010-12-01 CN CN2010105778478A patent/CN102485740A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1850846A (en) * | 2006-05-23 | 2006-10-25 | 辽宁百隆生物工程有限公司 | Production method for extracting chenodeoxycholic acid using chicken gall |
Non-Patent Citations (1)
| Title |
|---|
| SCALIA, S等: "Supercritical fluid extraction of bile acids from bovine bile raw materials", 《CHROMATOGRAPHIA》, vol. 48, no. 1112, 31 December 1998 (1998-12-31), pages 785 - 789 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103214538A (en) * | 2013-04-28 | 2013-07-24 | 广西北斗星动物保健品有限公司 | Method for separation and purification of bound total bile acid in bile paste |
| CN103214538B (en) * | 2013-04-28 | 2015-10-21 | 广西北斗星动物保健品有限公司 | The separation purification method of mating type total cholic acid in a kind of courage cream |
| CN105418715A (en) * | 2015-12-28 | 2016-03-23 | 成都市新功生物科技有限公司 | Method for extracting chenodeoxycholic acid by carbon dioxide supercritical extraction method |
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Application publication date: 20120606 |