CN111647025B - Method for extracting, separating and refining salicin from willow - Google Patents
Method for extracting, separating and refining salicin from willow Download PDFInfo
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- CN111647025B CN111647025B CN202010560448.4A CN202010560448A CN111647025B CN 111647025 B CN111647025 B CN 111647025B CN 202010560448 A CN202010560448 A CN 202010560448A CN 111647025 B CN111647025 B CN 111647025B
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Abstract
The invention relates to a method for extracting and separating refined salicin from willow, which relates to the technical field of extraction and separation, and comprises the steps of adding quicklime accounting for 8% of the weight of raw materials, fully and uniformly stirring, detecting the water content of the raw materials by a rapid instrument, and spraying a proper amount of water; reflux-extracting with 75% ethanol solution 7 times of the raw materials for two hours, and recovering extractive solution; recovering ethanol from the extractive solution under reduced pressure until no ethanol is present, and standing to room temperature to obtain salicin water solution; filtering the aqueous solution by dynamic cross flow through a membrane aperture 2 nanometer rotary ceramic membrane, and collecting filtrate; delivering the mixture into a refrigerating chamber for crystallization; separating by a release machine, collecting crystals, and drying to obtain crude crystals of salicin. The method can reduce alcohol consumption, save time and reduce production cost, and the salicin content of the prepared product can reach more than 99.5 percent.
Description
Technical Field
The invention relates to the technical field of extraction and separation, in particular to a method for extracting, separating and refining salicin from willows.
Background
Salicin, also known as salicin, is extracted from willow bark or branch, or by condensation of salicin and glucose. The salicin content in the willow bark or the willow branch is generally between 1.0 and 4.0 percent, and the main application is anti-inflammation, pain relieving and fever reducing. Salicin and aspirin (acetylsalicylic acid) have similar biological activity, have no irritation to stomach, and are not easy to cause gastrorrhagia. New research shows that it is an inhibitor of oxidase (NADH oxidase), has effects of resisting wrinkle, increasing skin luster and elasticity, reducing pigmentation, increasing skin moisture, etc., and has been applied in medicines, cosmetics, etc.
At present, the method for extracting salicin from willow barks or willow branches is more, and generally, the method comprises the steps of adding a proper amount of water into raw materials and alkaline substances (such as quicklime) to stir uniformly, extracting with alcohol or water, filtering the extracting solution, adsorbing the filtrate by macroporous adsorption resin, eluting by an organic solvent, crystallizing and other refining steps to obtain the finished product. The purity of the salicin can reach more than or equal to 98 percent, but no literature report that the purity of the salicin can reach 99.5 percent is available.
A process for extracting and separating salicin from red willow bark includes such steps as pulverizing red Pi Liuxian branch of small arbor, mixing with lime, stirring, laying aside for 30 min, extracting with alcohol for three times, recovering alcohol to obtain diluted extract, diluting with water, filtering, loading the supernatant to macroporous adsorption resin, merging the effluent with water, concentrating, laying aside for crystallizing, recrystallizing, suction filtering and vacuum drying. The process has the advantages that a large amount of ethanol is consumed during adsorption and elution, the cost is high, and the content cannot meet the production requirement of high-purity salicin.
Chinese patent CN1611508A (application number 200310105868. X) is a process for preparing salicin, which comprises the following steps: preparing materials, namely crushing willow branches and leaves into small-section raw materials; hydrolyzing and extracting, namely adding alkaline substances into the raw materials for hydrolysis, extracting by using an extractant, and removing residues; concentrating to obtain semi-finished product containing salicin, and refining to obtain salicin with purity not less than 95%. In the extraction process, a large amount of organic solvent is consumed, the cost is high, the environment is not protected, and the content cannot reach more than 98%.
For example, chinese patent CN102558254B is prepared with willow bark or fresh branch as material and through crushing, mixing with lime, stirring, setting for 30 min, water extraction, ultrafiltering, separating the filtrate with macroporous adsorption resin, mixing the effluent with water washing liquid, concentrating, setting for crystallization, decolorizing, re-crystallization and content up to 99%. The production process is complicated, ultrafiltration, adsorption and more technical control points are added, the product yield is not mentioned in the invention, and the production cost is high.
Disclosure of Invention
Aiming at the defects and shortcomings of the prior art, the invention provides a reasonable-design method for extracting, separating and refining salicin from willows, which can reduce alcohol consumption, save time and reduce production cost, and the salicin content of the prepared product can reach more than 99.5 percent.
In order to achieve the above purpose, the present invention adopts the following technical scheme: the operation steps are as follows:
1. taking Bai Liuliu bark or fresh willow branches as raw materials, and crushing the raw materials into 20-mesh small particles for later use;
2. adding quicklime accounting for 8% of the weight of the raw materials, fully and uniformly stirring, detecting the water content of the raw materials by a rapid instrument, spraying a proper amount of water, ensuring that the total water content of the raw materials reaches 55%, and piling and alkalizing for 240 minutes;
3. reflux-extracting with 75% ethanol solution 7 times of the raw materials for two hours, recovering extractive solution, reflux-extracting with 75% ethanol solution 5 times of the raw materials for one hour, collecting and mixing the two extractive solutions, and extracting for 3 hours with 12 times of the total solvent;
4. recovering ethanol from the extractive solution under reduced pressure until no ethanol is present, and standing to room temperature to obtain salicin water solution;
5. the water solution is dynamically filtered by cross flow through a rotary ceramic membrane with a membrane aperture of 2 nanometers, so that water and micromolecular substances pass through, macromolecular substances, microparticles, chlorophyll and bacteria are blocked by a filter membrane, the purposes of separation and purification are achieved, unfiltered liquid is discarded, and filtrate is collected;
6. concentrating the filtrate under negative pressure until the density is 1.18-1.2 g/cc, and collecting;
7. delivering the mixture into a refrigerating chamber for crystallization for 24 hours at the temperature of 4-10 ℃;
8. separating by a release machine, collecting crystals, and drying at 105 ℃ to obtain crude crystals of salicin, wherein the content of the crude crystals is 97% -98%;
9. the coarse crystallization is melted by 5 times of pure water, and after complete dissolution, the filtrate is moved into a refrigerating room for crystallization at 4-10 ℃ for 24 hours;
10. and (3) washing the centrifugal crystallization with cold water at 4-10 ℃ for 2 times, collecting the crystallization, and drying in vacuum at 75 ℃ to obtain a salicin finished product with the content of 99.7%.
The working principle of the invention is as follows: the water solution is filtered in a cross-flow mode through centrifugal force and hydraulic shearing force generated by the rotary motion of the rotary ceramic membrane with the membrane aperture of 2 nanometers and strong turbulence force of the aqueous solution of the salicin, so that water and molecular weight of the salicin (molecular weight of 18, molecular weight of the salicin of 286) completely pass through, macromolecular substances with molecular weight more than 400 and water insoluble particles such as protein, water-soluble polymer, chlorophyll, bacteria and the like are blocked by a filter membrane, and the purposes of separation and purification are achieved.
After the process is adopted, the beneficial effects of the invention are as follows: the invention provides a method for extracting, separating and refining salicin from willow, which adopts an aqueous solution to pass through a rotary ceramic membrane with the aperture of 2 nanometers, and adopts a dynamic cross-flow filtration ceramic membrane, and can greatly slow down membrane pollution and blockage by enabling a membrane component to rotate at a high speed; forcing all water molecules and salicin molecules (molecular weight is greater than 400) to pass through, and large molecular (molecular weight is greater than 400) substances and microparticles such as protein, water-soluble polymer, pigment, chlorophyll, bacteria and the like are blocked by a filter membrane, so that the purposes of separation and purification are achieved; the salicin content of the product obtained by the traditional twice crystallization process can reach 99.5%, decolorization is not needed, the yield is high, the cost is low, water and hexanol used in the production can be recycled, the pollution of an organic solvent to the environment is reduced, the process is simplified, and the industrialization is easy to realize.
Description of the drawings:
fig. 1 is a data chart of experiment one.
Fig. 2 is a data chart of experiment two.
The specific embodiment is as follows:
the following description of the embodiments of the present invention will be made clearly and completely with reference to the accompanying drawings, in which it is apparent that the embodiments described are only some embodiments of the present invention, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
The specific implementation mode adopts the following technical scheme: the operation steps are as follows:
1. taking Bai Liuliu bark or fresh willow branches as raw materials, and crushing the raw materials into 20-mesh small particles for later use;
2. adding quicklime accounting for 8% of the weight of the raw materials, fully and uniformly stirring, detecting the water content of the raw materials by a rapid instrument, spraying a proper amount of water, ensuring that the total water content of the raw materials reaches 55%, and piling and alkalizing for 240 minutes;
3. reflux-extracting with 75% ethanol solution 7 times of the raw materials for two hours, recovering extractive solution, reflux-extracting with 75% ethanol solution 5 times of the raw materials for one hour, collecting and mixing the two extractive solutions, and extracting for 3 hours with 12 times of the total solvent;
4. recovering ethanol from the extractive solution under reduced pressure until no ethanol is present, and standing to room temperature to obtain salicin water solution;
5. the water solution is dynamically filtered by cross flow through a rotary ceramic membrane with a membrane aperture of 2 nanometers, so that water and micromolecular substances pass through (the molecular weight is less than 400), macromolecular substances and microparticles (such as proteins, water-soluble polymers), chlorophyll, bacteria and the like are retained by a filter membrane, the purposes of separation and purification are achieved, unfiltered liquid is discarded, and filtrate is collected;
6. concentrating the filtrate under negative pressure (at a temperature of less than 75deg.C) to a density of 1.18-1.2 g/cc, and collecting;
7. delivering the mixture into a refrigerating chamber for crystallization for 24 hours at the temperature of 4-10 ℃;
8. separating by a release machine, collecting crystals, drying at 105 ℃, and (additionally treating mother liquor) obtaining crude crystals of salicin with the content of 97% -98%;
9. the coarse crystallization is melted by 5 times of pure water, and after complete dissolution, the filtrate is moved into a refrigerating room for crystallization at 4-10 ℃ for 24 hours;
10. and (3) washing the centrifugal crystallization with cold water at 4-10 ℃ for 2 times, collecting the crystallization, and drying in vacuum at 75 ℃ to obtain a salicin finished product with the content of 99.7%.
The working principle of the specific embodiment is as follows: the water solution is filtered in a cross-flow mode through centrifugal force and hydraulic shearing force generated by the rotary motion of the rotary ceramic membrane with the membrane aperture of 2 nanometers and strong turbulence force of the aqueous solution of the salicin, so that water and molecular weight of the salicin (molecular weight of 18, molecular weight of the salicin of 286) completely pass through, macromolecular substances with molecular weight more than 400 and water insoluble particles such as protein, water-soluble polymer, chlorophyll, bacteria and the like are blocked by a filter membrane, and the purposes of separation and purification are achieved.
After the process is adopted, the beneficial effects of the specific embodiment are as follows: the traditional membrane filtration salicin aqueous solution is static filtration, the flow rate of the liquid to be treated is increased by a pump to form cross-flow filtration, the pollution of a pollution blocking layer to the surface of a filtration membrane is prevented, the effective filtration time is short, the washing is frequent, 20% -30% of salicin is wrapped in a filtration membrane retaining phase, the product yield is seriously affected, and when high-viscosity precipitation is encountered at the bottom of the salicin aqueous solution, the method is low in efficiency and even not feasible. The specific implementation mode adopts an aqueous solution to pass through a pore diameter 2 nanometer rotary ceramic membrane, and a dynamic cross-flow filtration ceramic membrane is used, so that membrane pollution and blockage can be greatly slowed down by enabling a membrane component to rotate at a high speed; forcing all water molecules and salicin molecules (molecular weight is greater than 400) to pass through, and large molecular (molecular weight is greater than 400) substances and microparticles such as protein, water-soluble polymer, pigment, chlorophyll, bacteria and the like are blocked by a filter membrane, so that the purposes of separation and purification are achieved; the salicin content of the product obtained by the traditional twice crystallization process can reach 99.5%, decolorization is not needed, the yield is high, the cost is low, water and hexanol used in the production can be recycled, the pollution of an organic solvent to the environment is reduced, the process is simplified, and the industrialization is easy to realize.
Comparison experiment:
1000 kg of fresh white willow branches (with the tail end diameter smaller than 10MM and the raw material moisture content 38%) are collected in Jiang yanxiang bear north village (altitude 1700) in 3 months and 12 days in 2020. 1080L of aqueous solution is obtained after strictly pressing the steps 1 to 4, the density is 1.02 g/cc, and the temperature is 26 ℃. The salicin content of white willow bark extract was measured by RP-HPLC method (Hui Yuhu et al) Chinese herbal medicine 2004, volume 35 (stage 5), reference substance was salicin 99.8% marked by Shanghai Yuan Yew Biotech company. The salicin content in the aqueous solution is detected to be 26 g/L. This is referred to as stock solution in the following experiments.
Experiment one: the raw liquid is subjected to dynamic cross-flow filtration (with experimental serial numbers of 1, 2, 3 and 4) through the rotary ceramic membranes with membrane filtration areas of 2 square meters and membrane apertures of 1 nanometer, 2 nanometers, 3 nanometers and 4 nanometers respectively, and experimental data are shown in fig. 1, and as can be seen from fig. 1, the practical membrane aperture is the 2 nanometer ceramic membrane with the recovery rate of 95 percent, and the trapped macromolecule impurity amount is the largest.
Experiment II: after the filtrates of No. 1, no. 2, no. 3 and No. 4 obtained in the experiment are subjected to the steps 6 to 10 respectively, the obtained data are referred to fig. 2, and as can be seen from fig. 2, the total recovery rate of the aqueous solution crystallization after filtration by using the membrane pore size 2 nano ceramic membrane is 92%, and the product content is 98.7%.
Although the present invention has been described with reference to the foregoing embodiments, it will be apparent to those skilled in the art that modifications may be made to the embodiments described, or equivalents may be substituted for elements thereof, and any modifications, equivalents, improvements and changes may be made without departing from the spirit and principles of the present invention.
Claims (1)
1. A method for extracting, separating and refining salicin from willow is characterized in that: the operation steps are as follows:
(1) Taking Bai Liuliu bark or fresh willow branches as raw materials, and crushing the raw materials into 20-mesh small particles for later use;
(2) Putting quicklime accounting for 8% of the weight of the raw materials, fully and uniformly stirring, detecting the moisture of the raw materials by a rapid instrument, spraying a proper amount of water, ensuring the total moisture content of the raw materials to reach 55%, and piling and alkalizing for 240 minutes;
(3) Reflux-extracting with 75% ethanol solution 7 times of the raw materials for two hours, recovering the extractive solution, reflux-extracting with 75% ethanol solution 5 times of the extractive solution for one hour, collecting and mixing the two extractive solutions, and extracting for 3 hours with 12 times of the total solvent;
(4) Recovering ethanol from the extractive solution under reduced pressure until no ethanol is present, and standing to room temperature to obtain salicin water solution;
(5) The water solution is dynamically filtered by cross flow through a rotary ceramic membrane with a membrane aperture of 2 nanometers, so that water and micromolecular substances pass through, macromolecular substances, microparticles, chlorophyll and bacteria are blocked by a filter membrane, the purposes of separation and purification are achieved, unfiltered liquid is discarded, and filtrate is collected;
(6) Concentrating the filtrate to a density of 1.18-1.2 g/cc under negative pressure, and collecting;
(7) Delivering the mixture into a refrigerating chamber for crystallization for 24 hours at the temperature of 4-10 ℃;
(8) Separating by a centrifugal machine, collecting crystals, and drying at 105 ℃ to obtain coarse crystals of the salicin, wherein the content of the coarse crystals is 97% -98%;
(9) Performing heat dissolution on the crude crystals by using 5 times of pure water, and after complete dissolution, transferring filtrate into a refrigerating room for crystallization for 24 hours at 4-10 ℃;
(10) And (3) washing the centrifugal crystallization with cold water at 4-10 ℃ for 2 times, collecting the crystallization, and drying the crystallization in vacuum at 75 ℃ to obtain a salicin finished product with the content of 99.7%.
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Citations (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1554663A (en) * | 2003-12-29 | 2004-12-15 | 西安三江生物工程有限公司 | Process for extracting and separating salicin from fresh hranch of red willow |
| CN1611508A (en) * | 2003-10-30 | 2005-05-04 | 西安景行科技有限公司 | Process for preparing salicin |
| CN101117345A (en) * | 2007-08-29 | 2008-02-06 | 南京九思高科技有限公司 | Method for extracting stevioside |
| WO2008019941A1 (en) * | 2006-08-15 | 2008-02-21 | Henkel Ag & Co. Kgaa | Method for the separation and concentration of biomass |
| CN102020686A (en) * | 2009-09-17 | 2011-04-20 | 吴韬 | Method for preparing crystalline salicin from salicaceae plants |
| CN102558254A (en) * | 2010-12-30 | 2012-07-11 | 成都华高药业有限公司 | Extract of willow barks or willow branches and method for preparing salicin |
| CN102731587A (en) * | 2011-12-25 | 2012-10-17 | 大兴安岭林格贝有机食品有限责任公司 | Method for extracting salicin from white willow bark |
| CN105418807A (en) * | 2015-12-23 | 2016-03-23 | 青岛九龙生物医药有限公司 | Method for removing impurities in crude heparin sodium by using ceramic membrane |
| CN107488202A (en) * | 2017-07-21 | 2017-12-19 | 安徽龙津生物科技有限公司 | The extracting method in high yield of salicoside in a kind of white willow branches and leaves |
| CN107955051A (en) * | 2017-12-01 | 2018-04-24 | 吉首大学 | A kind of preparation method of aurantiin |
| CN109535209A (en) * | 2018-12-25 | 2019-03-29 | 中化健康产业发展有限公司 | A kind of process of the extraction purification stevioside from STEVIA REBAUDIANA |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| ITMI20051349A1 (en) * | 2005-07-14 | 2007-01-15 | Indena Spa | WILLOW EXTRACT USED AND FORMULATIONS THAT CONTAIN IT |
-
2020
- 2020-06-18 CN CN202010560448.4A patent/CN111647025B/en active Active
Patent Citations (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1611508A (en) * | 2003-10-30 | 2005-05-04 | 西安景行科技有限公司 | Process for preparing salicin |
| CN1554663A (en) * | 2003-12-29 | 2004-12-15 | 西安三江生物工程有限公司 | Process for extracting and separating salicin from fresh hranch of red willow |
| WO2008019941A1 (en) * | 2006-08-15 | 2008-02-21 | Henkel Ag & Co. Kgaa | Method for the separation and concentration of biomass |
| CN101117345A (en) * | 2007-08-29 | 2008-02-06 | 南京九思高科技有限公司 | Method for extracting stevioside |
| CN102020686A (en) * | 2009-09-17 | 2011-04-20 | 吴韬 | Method for preparing crystalline salicin from salicaceae plants |
| CN102558254A (en) * | 2010-12-30 | 2012-07-11 | 成都华高药业有限公司 | Extract of willow barks or willow branches and method for preparing salicin |
| CN102731587A (en) * | 2011-12-25 | 2012-10-17 | 大兴安岭林格贝有机食品有限责任公司 | Method for extracting salicin from white willow bark |
| CN105418807A (en) * | 2015-12-23 | 2016-03-23 | 青岛九龙生物医药有限公司 | Method for removing impurities in crude heparin sodium by using ceramic membrane |
| CN107488202A (en) * | 2017-07-21 | 2017-12-19 | 安徽龙津生物科技有限公司 | The extracting method in high yield of salicoside in a kind of white willow branches and leaves |
| CN107955051A (en) * | 2017-12-01 | 2018-04-24 | 吉首大学 | A kind of preparation method of aurantiin |
| CN109535209A (en) * | 2018-12-25 | 2019-03-29 | 中化健康产业发展有限公司 | A kind of process of the extraction purification stevioside from STEVIA REBAUDIANA |
Non-Patent Citations (4)
| Title |
|---|
| 丁启圣等编著.《新型实用过滤技术》.冶金工业出版社,2011,(第3版),第513-516页. * |
| 刘壮 ; 朱之 ; 漆虹.基于"絮凝-陶瓷膜耦合技术"的甜菊糖苷纯化工艺研究.《膜科学与技术》.2018,第38卷(第01期),第91-96页. * |
| 姚立霞.栀子黄色素提取及精制工艺的研究.《中国优秀硕士学位论文全文数据库 （工程科技Ⅰ辑）》.2009,(第9期),B024-103. * |
| 孔俊豪等.醇碱法提取胡杨叶水杨苷的工艺研究.《食品科技》.2012,第37卷(第37期),第205-209段. * |
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