CN110627857A - Environment-friendly method for removing oil in animal bile - Google Patents
Environment-friendly method for removing oil in animal bile Download PDFInfo
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- CN110627857A CN110627857A CN201910993407.1A CN201910993407A CN110627857A CN 110627857 A CN110627857 A CN 110627857A CN 201910993407 A CN201910993407 A CN 201910993407A CN 110627857 A CN110627857 A CN 110627857A
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- 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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Abstract
The invention belongs to the technical field of medicine preparation, and discloses an environment-friendly method for removing oil in animal bile, which comprises the following steps: 1) preparing animal bile; 2) preparing an adsorption layer: tiling a silicon dioxide layer with the thickness of 8cm, tiling an iron oxide layer with the thickness of 3cm on the silicon dioxide layer, and tiling an aluminum oxide layer with the thickness of 5cm on the iron oxide layer; compacting the paving layer to prepare the adsorption layer; 3) removing oil in animal bile: leaking animal bile by using the adsorption layer until the reduction of the oil content in the leaking liquid to the oil content in the animal bile is more than 80 percent; 4) regeneration of the adsorption layer: and (3) carrying out leakage regeneration on the adsorption layer by adopting ethanol, recycling the regenerated adsorption layer, and concentrating leaked mother liquor to be dry to obtain the grease base material. The method has simple facilities, controllable operation and high oil removal rate, and can improve the yield and purity of chenodeoxycholic acid by removing animal bile oil by the method.
Description
Technical Field
The invention belongs to the technical field of medicine preparation, and particularly relates to an environment-friendly method for removing oil in animal bile.
Background
The animal bile is juice extracted from animal gallbladder, has bitter taste, is used for eliminating toxic heat, discharging fire and qi, eliminating phlegm, relieving cough, regulating blood lipid and blood pressure, relieving fatigue, and inhibiting acute and chronic inflammation. Because of its many effects, it is currently used in clinical practice in a particularly wide range, for example: treating pertussis, chronic tracheitis, hemorrhoid, etc.
The animal bile mainly contains Chenodeoxycholic acid (CDCA), Chenodeoxycholic acid (Chenodeoxycholic acid), 3 alpha, 7 alpha-dihydroxy-5-beta-cholanic acid (CDCA), and C24H40O4Molecular weight 392.57. Chenodeoxycholic acid has pharmacological effects of promoting secretion of bile and bile salt, dissolving cholelithiasis, enhancing activity of pancreatic lipase, promoting digestion of fat by pancreatic lipase, relieving inflammation, relieving cough, and resisting hypertension.
When the chenodeoxycholic acid is extracted from the animal bile, because the animal bile contains a large amount of grease, if the grease is not removed by an effective method, the yield of the chenodeoxycholic acid extracted from the animal bile is greatly reduced, and the extraction amount of the chenodeoxycholic acid cannot be increased. At present, gasoline, n-heptane and petroleum ether are adopted to remove the oil in the animal bile, the removal effect is poor, the removal rate can only reach 40%, and the gasoline and the petroleum ether belong to organic solvents, and the volatilization of the gasoline and the petroleum ether can pollute the environment. For example: patent document CN200610046652.4 uses equal amount of 120 # gasoline to remove grease. Patent document CN201610036123.X adopts n-heptane and diluted hydrochloric acid to adjust pH to 2-3 to remove oil and fat. Patent document CN201310092280.9 adopts the addition of petroleum ether to remove grease.
Disclosure of Invention
In view of the above problems in the prior art, the present invention is directed to an environment-friendly method for removing oil from animal bile. The method has the advantages of simple facility, simple and controllable operation and high oil removal rate, and can improve the yield and purity of chenodeoxycholic acid extracted from animal bile after the oil in the animal bile is removed by the method.
The invention provides an environment-friendly method for removing oil in animal bile, which comprises the following steps:
1) preparing animal bile;
2) preparing an adsorption layer: tiling a silicon dioxide layer with the thickness of 8cm, tiling an iron oxide layer with the thickness of 3cm on the silicon dioxide layer, and tiling an aluminum oxide layer with the thickness of 5cm on the iron oxide layer; compacting the paving layer to prepare the adsorption layer;
3) removing oil in animal bile: leaking animal bile by using the adsorption layer until the reduction of the oil content in the leaking liquid to the oil content in the animal bile is more than 80 percent;
4) regeneration of the adsorption layer: and (3) carrying out leakage regeneration on the adsorption layer by adopting ethanol, recycling the regenerated adsorption layer, and concentrating leaked mother liquor to be dry to obtain a grease base material which is used as a raw material of a biomass diesel workshop.
In the present invention, the animal bile can be prepared by a conventional method in the prior art, and preferably, the step 1) comprises: crushing animal bile, heating at 40 deg.C for 15min, and filtering to obtain animal bile.
Preferably, in the step 2), a jack of 100 tons is adopted to apply pressure to the paving layer, and the pressure is maintained for 1 hour under the pressure of 0.5 MPa.
According to the invention, the oil content is detected by adopting a thin-layer chromatography, wherein a chromatographic agent comprises dichloromethane, acetic acid and ethanol with the volume ratio of 5: 2: 3, and a color developing agent is 5wt% of sulfuric acid ethanol solution.
Preferably, in step 3), the animal bile is leaked at least once by using the adsorption layer, and a new or regenerated adsorption layer is used for each leakage. And after each leakage, detecting the content of the oil in the leakage liquid, and compared with the oil content in the animal bile, if the oil content is reduced by less than 80%, removing the oil from the leakage liquid by using a new or regenerated adsorption layer until the oil content is reduced by more than 80%.
Preferably, in the step 4), the amount of ethanol is 10 times of the content (by mass) of the oil in the adsorption layer.
The technological parameters which are not limited in the invention are carried out by adopting the conventional mode in the field, such as the detection, concentration and the like of the oil content.
Compared with the prior art, the invention has the following beneficial effects:
1. the invention adopts the adsorption layer consisting of the silicon dioxide layer, the ferric oxide layer and the aluminum oxide layer to adsorb the grease in the animal bile, the grease removal rate can reach 80 percent, and the invention has no pollution and high adsorption efficiency.
2. After the animal bile is degreased by the method, the yield of the chenodeoxycholic acid extracted from the animal bile can be improved by 150 percent (for example, the yield of the chicken bile is improved to 2.5 percent from 1 percent of the traditional process), the purity of the extracted chenodeoxycholic acid can reach 98.29 percent, and the beneficial effect is very obvious.
3. The invention adopts the ethanol leakage method to regenerate the adsorption layer for repeated reuse, thereby not only protecting the environment, but also saving the production cost, improving the profit of manufacturers, and simultaneously recycling the grease.
4. The method can be used for removing grease in bile of various animals such as chicken, duck, goose, pig, sheep and the like, and has obvious effect.
Drawings
FIG. 1: chromatogram of chenodeoxycholic acid obtained in example 1.
Detailed Description
The technical solutions of the present invention will be described clearly and completely with reference to the following embodiments of the present invention, and it should be understood that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments.
Examples 1-2 are intended to illustrate the environmentally friendly method of removing oil from animal bile according to the present invention.
Example 1
An environment-friendly method for removing oil in chicken bile comprises the following steps:
1) preparing chicken bile: crushing chicken gallbladder, heating at 40 deg.C for 15min, and filtering to obtain chicken bile;
2) preparing an adsorption layer: tiling a silicon dioxide layer with the thickness of 8cm, tiling an iron oxide layer with the thickness of 3cm on the silicon dioxide layer, and tiling an aluminum oxide layer with the thickness of 5cm on the iron oxide layer; applying pressure to the paving layer by adopting a jack of 100 tons, maintaining the pressure for 1 hour under the pressure of 0.5MPa, and compacting the paving layer to obtain the adsorption layer;
3) removing oil in the chicken bile: the chicken bile is leaked by adopting the adsorption layer, a new or regenerated adsorption layer is adopted for each leakage, after each leakage, the content of the oil in the leakage liquid is detected (the oil content is detected by adopting a thin-layer chromatography, a chromatographic agent adopts dichloromethane, acetic acid and ethanol with the volume ratio of 5: 2: 3, and a color developing agent is a 5wt% ethanol sulfate solution), and the leakage is performed for 2 times, so that the reduction of the oil content in the obtained leakage liquid is 80% compared with the oil content in the chicken bile;
4) regeneration of the adsorption layer: and (3) carrying out leakage regeneration on the adsorption layer by adopting ethanol, wherein the using amount of the ethanol is 10 times of the content (mass) of the grease in the adsorption layer, the regenerated adsorption layer is recycled, and the leaked mother liquor is concentrated to be dry to obtain a grease base material which is used as a raw material of a biomass diesel workshop.
Extracting chenodeoxycholic acid from chicken bile without oil by conventional method with yield of 2.5% and purity of obtained chenodeoxycholic acid of 98.292%, and chromatogram thereof is shown in figure 1.
Example 2
An environment-friendly method for removing grease in pig bile comprises the following steps:
1) preparing pig bile: crushing fel Sus Domestica, heating at 40 deg.C for 15min, and filtering to obtain fel Sus Domestica;
2) preparing an adsorption layer: tiling a silicon dioxide layer with the thickness of 8cm, tiling an iron oxide layer with the thickness of 3cm on the silicon dioxide layer, and tiling an aluminum oxide layer with the thickness of 5cm on the iron oxide layer; applying pressure to the paving layer by adopting a jack of 100 tons, maintaining the pressure for 1 hour under the pressure of 1MPa, and compacting the paving layer to obtain the adsorption layer;
3) removing grease in the pig bile: the pig bile is leaked by adopting the adsorption layer, a new or regenerated adsorption layer is adopted for each leakage, after each leakage, the content of the grease in the leakage liquid is detected (the grease content is detected by adopting a thin-layer chromatography, a chromatographic agent adopts dichloromethane, acetic acid and ethanol with the volume ratio of 5: 2: 3, and a color developing agent is a 5wt% ethanol sulfate solution), and the leakage is performed for 2 times, wherein the reduction of the grease content in the obtained leakage liquid to the grease content in the pig bile is 80%;
4) regeneration of the adsorption layer: and (3) carrying out leakage regeneration on the adsorption layer by adopting ethanol, wherein the using amount of the ethanol is 10 times of the content (mass) of the grease in the adsorption layer, the regenerated adsorption layer is recycled, and the leaked mother liquor is concentrated to be dry to obtain a grease base material which is used as a raw material of a biomass diesel workshop.
Extracting chenodeoxycholic acid from the fat-removed pig bile by a conventional method, wherein the yield is 0.8%, and the purity of the obtained chenodeoxycholic acid is 98.2%.
Comparative example 1
The fat of the chicken bile in example 1 was removed by a conventional method, 1 time of petroleum ether was added to the chicken bile, and the mixture was stirred at 40 ℃ for 1 hour to separate layers, the upper layer was a petroleum ether layer (fat), the lower layer was the fat-removed chicken bile, and the amount of the fat content in the fat-removed chicken bile was reduced by 50%. Chenodeoxycholic acid was extracted by a conventional method (same as example 1) to obtain chenodeoxycholic acid with a purity of 80% and a yield of only 1% according to chicken bile.
Comparative example 2
Removing grease from the pig bile in example 2 by a conventional method, heating the pig bile to 40 ℃, standing for 2 hours, partitioning an upper grease layer, cooling to 10 ℃, and filtering by using a 30-mesh filter screen to obtain the grease-removed pig bile, wherein the reduction amount of the grease content in the grease-removed pig bile is 60%. The chenodeoxycholic acid was extracted by a conventional method (same as example 2) to obtain chenodeoxycholic acid with a purity of 82% and a yield of 0.4%.
Compared with the comparative example 1, the yield of the extracted chenodeoxycholic acid of the chicken bile treated by the method disclosed by the invention is improved to 2.5% from 1% of that of the traditional process, and the purity of the extracted chenodeoxycholic acid is improved to 98.292% from 80%; comparing example 2 with comparative example 2, the yield of chenodeoxycholic acid extracted from the pig bile treated by the method of the invention is improved to 0.8% from 0.4% of the traditional process, and the purity of the extracted chenodeoxycholic acid is improved to 98.2% from 82%.
Having described embodiments of the present invention, the foregoing description is intended to be exemplary, not exhaustive, and not limited to the disclosed embodiments. Many modifications and variations will be apparent to those of ordinary skill in the art without departing from the scope and spirit of the illustrated embodiments.
Claims (6)
1. An environment-friendly method for removing oil in animal bile is characterized by comprising the following steps:
1) preparing animal bile;
2) preparing an adsorption layer: tiling a silicon dioxide layer with the thickness of 8cm, tiling an iron oxide layer with the thickness of 3cm on the silicon dioxide layer, and tiling an aluminum oxide layer with the thickness of 5cm on the iron oxide layer; compacting the paving layer to prepare the adsorption layer;
3) removing oil in animal bile: leaking animal bile by using the adsorption layer until the reduction of the oil content in the leaking liquid to the oil content in the animal bile is more than 80 percent;
4) regeneration of the adsorption layer: and (3) carrying out leakage regeneration on the adsorption layer by adopting ethanol, recycling the regenerated adsorption layer, and concentrating leaked mother liquor to be dry to obtain a grease base material which is used as a raw material of a biomass diesel workshop.
2. The environment-friendly method for removing oil from animal bile according to claim 1, wherein the method comprises the following steps: the step 1) comprises the following steps: crushing animal bile, heating at 40 deg.C for 15min, and filtering to obtain animal bile.
3. The environment-friendly method for removing oil from animal bile according to claim 1, wherein the method comprises the following steps: in the step 2), a 100-ton jack is adopted to press the paving layer, and the pressure is maintained for 1h under the pressure of 0.5-1 MPa.
4. The environment-friendly method for removing oil from animal bile according to claim 1, wherein the method comprises the following steps: detecting oil content by thin layer chromatography, wherein the chromatographic agent is dichloromethane, acetic acid and ethanol with volume ratio of 5: 2: 3, and the developer is 5wt% sulphuric acid ethanol solution.
5. The environment-friendly method for removing oil from animal bile according to claim 1, wherein the method comprises the following steps: in the step 3), the animal bile leaks at least once by adopting the adsorption layer, and a new or regenerated adsorption layer is adopted for each leakage.
6. The environment-friendly method for removing oil from animal bile according to claim 1, wherein the method comprises the following steps: in the step 4), the dosage of the ethanol is 10 times of the content of the oil in the adsorption layer.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104311620A (en) * | 2014-09-26 | 2015-01-28 | 上海分普新材料科技有限公司 | Method for purifying chenodeoxycholic acid |
| CN105481926A (en) * | 2015-12-25 | 2016-04-13 | 成都市新功生物科技有限公司 | Method for directly preparing chenodeoxycholic acid from duck bile |
| 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 |
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- 2019-10-18 CN CN201910993407.1A patent/CN110627857A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104311620A (en) * | 2014-09-26 | 2015-01-28 | 上海分普新材料科技有限公司 | Method for purifying chenodeoxycholic acid |
| CN105481926A (en) * | 2015-12-25 | 2016-04-13 | 成都市新功生物科技有限公司 | Method for directly preparing chenodeoxycholic acid from duck bile |
| 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 |
Non-Patent Citations (1)
| Title |
|---|
| 王沛: "《全国中医药行业高等教育"十三五"规划教材 制药工艺学》", 31 December 2017 * |
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Application publication date: 20191231 |