CN102167717A - Method for extracting cholesterol from animal brain dry powder with ultrasonic waves - Google Patents
Method for extracting cholesterol from animal brain dry powder with ultrasonic waves Download PDFInfo
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- CN102167717A CN102167717A CN 201110050728 CN201110050728A CN102167717A CN 102167717 A CN102167717 A CN 102167717A CN 201110050728 CN201110050728 CN 201110050728 CN 201110050728 A CN201110050728 A CN 201110050728A CN 102167717 A CN102167717 A CN 102167717A
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Abstract
The invention relates to a method for extracting cholesterol from animal brain dry powder with ultrasonic waves. Animal brain dry powder is used as raw materials, and the method comprises the steps of: I, dipping before extraction; II, ultrasonic extraction; III, concentration and recovery of acetone; IV, hydrolysis, cooling and crystallization; V, dissolution and crystallization; VI, recrystallization; and VII making of finished products. The method has the advantages that first, the used quantity of a dipping solution for the animal brain dry powder is reduced (5 times of quantity is used to the largest); second, the dipping time is enormously shortened (the dipping lasts for 9h furthest); third, high-purity cholesterol (with purity of 95%-97%) can be obtained by three times of crystallization on the premise of guaranteeing high yield (up to 8.5%-10%), and multiple reflux and heating ensure no toxic organic solvent left.
Description
Technical field
The present invention relates to the extracting process of effective constituent in the animal brain, relate in particular to a kind of method of utilizing cholesterol in the ultrasonic extraction animal brain dry powder.
Background technology
Containing multiple abundant material in animal (pig, ox, sheep etc.) the brain stem powder composition, major ingredient is the important source material of medicine, makeup, liquid crystal material, feeding additive aquatic animal in the contained material, how to extract effective ingredient fully, become the key point that to utilize.Conventional art adopts the acetone extract method to extract cholesterol from animal brain stem powder, this method adds 10 times of amount acetone solns in animal brain dry powder, flood length consuming time (nearly 72 hours), extraction cholesterol yield low (＜6%), purity low (≤90%), and residual poisonous organic solvent, institute's extracting substance can only be used for fodder additives, causes the animal brain resource to waste.
Summary of the invention
The objective of the invention is in order to solve the deficiency of said extracted method, a kind of method of utilizing cholesterol in the ultrasonic extraction animal brain dry powder is provided, realization extracts highly purified cholesterol from animal brain stem powder, this method has yield height, short, the bio-transformation efficient height of flow process, does not have characteristics such as poisonous organic solvent residual.
For achieving the above object, the technical scheme taked of the present invention is:
A kind of method of utilizing cholesterol in the ultrasonic extraction animal brain dry powder, its step is as follows: 1, the dipping before the extraction, in animal brain dry powder, add the acetone soln that it measures 3～5 times, make animal brain dry powder in solution, fully flood dipping time 7～9 hours; 2, ultrasonic extraction is with the animal brain dry powder behind the dipping and the mixture of acetone soln, in the ultrasonic extraction still of packing into, with the ultrasonic emitting frequency setting at 30～50KHz, temperature regulation is controlled at 25～35 ℃, 5～15 minutes extraction time, filters and obtains extraction liquid; 3, concentrate recovery acetone, extraction liquid is put into thickener, set thickener vacuum tightness 0.06～0.08Mpa, 35～40 ℃ of temperature, acetone is reclaimed in the recirculated water cooling, obtains yellow paste; 4, hydrolysis crystallisation by cooling, the ethanolic soln that in the yellow paste that obtains, adds 4～6 times of amount concentration 93～97%, add acid and adjust pH value, make pH value reach at 1.5～3 o'clock, put into thickener reflux dissolving 30～100 minutes, set 75～80 ℃ of the interior temperature of thickener, after the filtration filtrate is placed crystallisation by cooling under the normal temperature, obtain xln and be crude product cholesterol crystal body; 5, dissolving crystallized, the ethanolic soln that in crude product cholesterol crystal body, adds 8～10 times of amounts 93～97%, processing industry alkali is adjusted pH value, make pH value reach at 10～13 o'clock, put into thickener reflux dissolving 30～40 minutes, set 75～80 ℃ of the interior temperature of thickener, after the filtration filtrate is placed crystallisation by cooling under the normal temperature, obtain xln and be thick cholesterol crystal body; 6, recrystallization, the ethanolic soln that in thick cholesterol crystal body, adds 8～10 times of amounts 93～97%, put into the thickener reflux 50～60 minutes, set 75～80 ℃ of the interior temperature of thickener, keep filtering under the temperature-resistant situation, with crystallisation by cooling under the filtrate normal temperature, obtain xln and be elaboration cholesterol crystal body; 7, make finished product, elaboration cholesterol crystal body is put into vacuum drying oven, set vacuum tightness 0.06～0.08Mpa in the vacuum drying oven, 80～85 ℃ of temperature, vacuum-drying obtains the finished product cholesterol after 2 hours.
The present invention uses ultrasonic wave in the process of extraction, will treat that extracting substance is separated in the extraction liquid fully, utilizes thickener to concentrate and reclaims acetone soln, and dipping solution is effectively utilized; Compared with the prior art, beneficial effect of the present invention is: the usage quantity (traditional method is used 10 times of amounts of acetone soln, and the present invention uses acetone soln to be 5 times of amounts to the maximum) that 1, has reduced animal brain stem dipping solution; 2, shortened dipping time (traditional method was flooded 72 hours consuming time, 9 hours consuming time of the longest dipping of the present invention) greatly; 3, guaranteed to obtain the cholesterol of high purity (purity reaches 95%～99%) under the situation of high yield (yield reaches 8.5%～12%) by three crystallisation processs, and repeatedly refluxed and heat and guaranteed no poisonous organic solvent residual (the acetone boiling temperature is 56 ℃).
Embodiment:
Below in conjunction with specific embodiment the present invention is described in further details.
Embodiment 1
When laboratory lab scale or sampling experiment, get animal brain dry powder 0.1kg and put into experimental ware, add the acetone soln of 3 times of amounts, allow animal brain dry powder in acetone soln, flood 7 hours, it is fully flooded;
With the animal brain dry powder behind the dipping and the mixture of acetone soln, pack in the ultrasonic extraction still, set the ultrasonic emitting frequency 30～40KHz of ultrasonic extraction still, 25～28 ℃ of temperature, extracted 5～10 minutes, can guarantee farthest to extract cholesterol, use special-purpose sheet frame to filter, can obtain the extraction liquid of follow-up use;
Extraction liquid is put into Rotary Evaporators, set Rotary Evaporators vacuum tightness 0.06Mpa, 39～40 ℃ of temperature, acetone is reclaimed in the recirculated water cooling, obtains yellow paste;
Take out yellow paste, the ethanolic soln that in the vessel of yellow paste are housed, adds 4 times of amount concentration 96～97%, add hydrochloric acid and adjust pH value, when pH value reaches 2.5～3, put into water-bath reflux dissolving 30～40 minutes, set 79～80 ℃ of water-bath kettle temperatures, use filter cloth to filter, filtrate is placed crystallisation by cooling under the normal temperature, obtain xln and be crude product cholesterol crystal body;
The ethanolic soln that in the container that crude product cholesterol body is housed, adds 8 times of amounts 96～97%, processing industry alkali is adjusted pH value, make pH value reach at 12～13 o'clock, put into water-bath reflux dissolving 30～32 minutes, set 79～80 ℃ of water-bath kettle temperatures, use filter cloth to filter, filtrate is placed crystallisation by cooling under the normal temperature, obtain xln and be thick cholesterol crystal body, the parameter setting of ethanol, pH value and reflux has guaranteed the cholesterol sufficient crystallising in this project, improve the yield of cholesterol, guaranteed to extract the purity of cholesterol;
The ethanolic soln that in the container that thick cholesterol crystal body is housed, adds 8 times of amounts 96～97%, put into the water-bath reflux 50～55 minutes, set 79～80 ℃ of water-bath kettle temperatures, keep filtering under the temperature-resistant situation, filtrate is placed crystallisation by cooling under the normal temperature, obtain xln and be elaboration cholesterol crystal body, the parameter that relates in this project has effectively guaranteed to extract the purity of cholesterol;
Elaboration cholesterol crystal body is put into vacuum drying oven, set 80～82 ℃ of vacuum drying oven temperature, set vacuum tightness 0.08Mpa, both got finished product after dry 2 hours.
Embodiment 2
In process of production, get animal brain dry powder 10kg and put into experimental ware, add the acetone soln of 5 times of amounts this moment, allows animal brain dry powder flood in acetone soln 9 hours, and it is fully flooded;
The experimental ware that solution is housed is put into the ultrasonic extraction still, set the ultrasonic emitting frequency 40～50KHz of ultrasonic extraction still, 30～35 ℃ of temperature, extracted 10～15 minutes, filter with special-purpose sheet frame then, obtain extraction liquid, this process has effectively guaranteed the yield of cholesterol;
Extraction liquid is put into spherical thickener, set spherical thickener vacuum tightness 0.08Mpa, 35～37 ℃ of design temperatures, acetone is reclaimed in the recirculated water cooling, obtains yellow paste;
With the yellow paste vessel of packing into, the ethanolic soln that in the vessel of yellow paste are housed, adds 6 times of amount concentration 93～95%, add hydrochloric acid and adjust pH value, when pH value reaches 1.5～2, put into spherical thickener reflux dissolving 60～100 minutes, set 75～77 ℃ of the interior temperature of spherical thickener, use filter cloth to filter, filtrate is placed crystallisation by cooling under the normal temperature, obtain xln and be crude product cholesterol crystal body;
The ethanolic soln that in the container that crude product cholesterol crystal body is housed, adds 10 times of amounts 93～95%, processing industry alkali is adjusted pH value, make pH value reach at 10～11 o'clock, put into spherical thickener reflux dissolving 35～40 minutes, set 75～77 ℃ of the interior temperature of spherical thickener, use filter cloth to filter, filtrate is placed crystallisation by cooling under the normal temperature, obtain xln and be thick cholesterol crystal body, the parameter setting of ethanol, pH value and reflux has guaranteed the cholesterol sufficient crystallising in this project, improve the yield of cholesterol, guaranteed to extract the purity of cholesterol;
The ethanolic soln that in the container that thick cholesterol crystal body is housed, adds 10 times of amounts 93～95%, put into spherical thickener reflux dissolving 58～60 minutes, set 75～77 ℃ of the interior temperature of spherical thickener, keep under the temperature-resistant situation, use the titanium rod to filter, with crystallisation by cooling under the filtrate normal temperature, obtain xln and be elaboration cholesterol crystal body, the parameter that relates in this project has effectively guaranteed to extract the purity of cholesterol;
Elaboration cholesterol crystal body is put into vacuum drying oven, set 83～85 ℃ of vacuum drying oven temperature, set vacuum tightness 0.06～0.07Mpa, both got finished product after dry 2 hours.
Because the difference that reaches vacuum apparatus that concentrates used in the present invention, can produce the adjustment of parameter areas such as temperature, usage quantity, pH value, vacuum tightness, but the above parameter of experimental result all in the normal range that the present invention provides, therefore no longer provides too much embodiment.
Claims (7)
1. method of utilizing cholesterol in the ultrasonic extraction animal brain dry powder, it is characterized in that: step is as follows: 1, the dipping before the extraction, the acetone soln that adds 3～5 times of its amounts in animal brain dry powder makes animal brain dry powder fully flood dipping time 7～9 hours in solution; 2, ultrasonic extraction is with the animal brain dry powder behind the dipping and the mixture of acetone soln, in the ultrasonic extraction still of packing into, with the ultrasonic emitting frequency setting at 30～50KHz, temperature regulation is controlled at 25～35 ℃, 5～15 minutes extraction time, filters and obtains extraction liquid; 3, concentrate recovery acetone, extraction liquid is put into thickener, set thickener vacuum tightness 0.06～0.08Mpa, 35～40 ℃ of temperature, acetone is reclaimed in the recirculated water cooling, obtains yellow paste; 4, hydrolysis crystallisation by cooling, the ethanolic soln that in the yellow paste that obtains, adds 4～6 times of amount concentration 93～97%, add acid and adjust pH value, make pH value reach at 1.5～3 o'clock, put into thickener reflux dissolving 30～100 minutes, set 75～80 ℃ of the interior temperature of thickener, after the filtration filtrate is placed crystallisation by cooling under the normal temperature, obtain xln and be crude product cholesterol crystal body; 5, dissolving crystallized, the ethanolic soln that in crude product cholesterol crystal body, adds 8～10 times of amounts 93～97%, processing industry alkali is adjusted pH value, make pH value reach at 10～13 o'clock, put into thickener reflux dissolving 30～40 minutes, set 75～80 ℃ of the interior temperature of thickener, after the filtration filtrate is placed crystallisation by cooling under the normal temperature, obtain xln and be thick cholesterol crystal body; 6, recrystallization, the ethanolic soln that in thick cholesterol crystal body, adds 8～10 times of amounts 93～97%, put into the thickener reflux 50～60 minutes, set 75～80 ℃ of the interior temperature of thickener, keep filtering under the temperature-resistant situation, with crystallisation by cooling under the filtrate normal temperature, obtain xln and be elaboration cholesterol crystal body; 7, make finished product, elaboration cholesterol crystal body is put into vacuum drying oven, set vacuum tightness 0.06～0.08Mpa in the vacuum drying oven, 80～85 ℃ of temperature, vacuum-drying obtains the finished product cholesterol after 2 hours.
2. the method for utilizing cholesterol in the ultrasonic extraction animal brain dry powder according to claim 1 is characterized in that: in the ultrasonic extraction process, set the ultrasonic emitting frequency 30～40KHz of ultrasonic extraction still, 25～28 ℃ of temperature extracted 5～10 minutes.
3. the method for utilizing cholesterol in the ultrasonic extraction animal brain dry powder according to claim 1 is characterized in that: in the ultrasonic extraction process, set the ultrasonic emitting frequency 40～50KHz of ultrasonic extraction still, 30～35 ℃ of temperature extracted 10～15 minutes.
4. the method for utilizing cholesterol in the ultrasonic extraction animal brain dry powder according to claim 1, it is characterized in that: the ethanolic soln that in the container that crude product cholesterol crystal body is housed, adds 8 times of amounts 96～97% in the dissolving crystallized process, processing industry alkali is adjusted pH value, make pH value reach at 12～13 o'clock, put into water-bath reflux dissolving 30～32 minutes, set 79～80 ℃ of water-bath kettle temperatures.
5. the method for utilizing cholesterol in the ultrasonic extraction animal brain dry powder according to claim 1, it is characterized in that: the ethanolic soln that in the container that crude product cholesterol crystal body is housed, adds 10 times of amounts 93～95% in the dissolving crystallized process, processing industry alkali is adjusted pH value, make pH value reach at 10～11 o'clock, put into spherical thickener reflux dissolving 35～40 minutes, set 75～77 ℃ of the interior temperature of spherical thickener.
6. the method for utilizing cholesterol in the ultrasonic extraction animal brain dry powder according to claim 1, it is characterized in that: the ethanolic soln that in the container that thick cholesterol crystal body is housed, adds 8 times of amounts 96～97% in the recrystallization process, put into the water-bath reflux 50～55 minutes, and set 79～80 ℃ of water-bath kettle temperatures.
7. the method for utilizing cholesterol in the ultrasonic extraction animal brain dry powder according to claim 1, it is characterized in that: the ethanolic soln that in the container that thick cholesterol crystal body is housed, adds 10 times of amounts 93～95% in the recrystallization process, put into spherical thickener reflux dissolving 58～60 minutes, set 75～77 ℃ of the interior temperature of spherical thickener.
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| CN 201110050728 CN102167717B (en) | 2011-02-22 | 2011-02-22 | Method for extracting cholesterol from animal brain dry powder with ultrasonic waves |
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| CN 201110050728 CN102167717B (en) | 2011-02-22 | 2011-02-22 | Method for extracting cholesterol from animal brain dry powder with ultrasonic waves |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103804449A (en) * | 2012-11-14 | 2014-05-21 | 石汉生 | Preparation process of cholesterol |
| CN107141331A (en) * | 2017-07-07 | 2017-09-08 | 赵厚发 | The extracting method of cholesterol in a kind of marine organisms byproduct |
| CN109180766A (en) * | 2018-09-12 | 2019-01-11 | 四川奇格曼药业有限公司 | A kind of extraction cholesterol technique |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| RU2034552C1 (en) * | 1993-01-11 | 1995-05-10 | Николай Викторович Ильинков | Method for obtaining cholesterol from brain tissue |
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2011
- 2011-02-22 CN CN 201110050728 patent/CN102167717B/en not_active Expired - Fee Related
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| RU2034552C1 (en) * | 1993-01-11 | 1995-05-10 | Николай Викторович Ильинков | Method for obtaining cholesterol from brain tissue |
Non-Patent Citations (2)
| Title |
|---|
| 《中国生化药物杂志》 19900131 戴星 陈蒙熙 胆固醇提取工艺探讨 第44－46页 1－7 , 第1期 * |
| 《北方牧业》 20030515 凡人 胆固醇的提取工艺 第25页 1－7 , 第9期 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103804449A (en) * | 2012-11-14 | 2014-05-21 | 石汉生 | Preparation process of cholesterol |
| CN107141331A (en) * | 2017-07-07 | 2017-09-08 | 赵厚发 | The extracting method of cholesterol in a kind of marine organisms byproduct |
| CN109180766A (en) * | 2018-09-12 | 2019-01-11 | 四川奇格曼药业有限公司 | A kind of extraction cholesterol technique |
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| CN102167717B (en) | 2012-12-05 |
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