CN113603734A - Method for extracting salidroside - Google Patents
Method for extracting salidroside Download PDFInfo
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- CN113603734A CN113603734A CN202110921820.4A CN202110921820A CN113603734A CN 113603734 A CN113603734 A CN 113603734A CN 202110921820 A CN202110921820 A CN 202110921820A CN 113603734 A CN113603734 A CN 113603734A
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- extracting
- extraction
- salidroside
- tank body
- extraction device
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- 238000000034 method Methods 0.000 title claims abstract description 25
- ILRCGYURZSFMEG-UHFFFAOYSA-N Salidroside Natural products OC1C(O)C(O)C(CO)OC1OCCC1=CC=C(O)C=C1 ILRCGYURZSFMEG-UHFFFAOYSA-N 0.000 title claims abstract description 21
- ILRCGYURZSFMEG-RQICVUQASA-N salidroside Chemical compound O[C@@H]1[C@@H](O)[C@H](O)[C@@H](CO)OC1OCCC1=CC=C(O)C=C1 ILRCGYURZSFMEG-RQICVUQASA-N 0.000 title claims abstract description 21
- 238000000605 extraction Methods 0.000 claims abstract description 51
- 239000011347 resin Substances 0.000 claims abstract description 26
- 229920005989 resin Polymers 0.000 claims abstract description 26
- 238000001914 filtration Methods 0.000 claims abstract description 8
- 239000012528 membrane Substances 0.000 claims abstract description 8
- 238000001728 nano-filtration Methods 0.000 claims abstract description 8
- 238000001035 drying Methods 0.000 claims abstract description 3
- 238000003756 stirring Methods 0.000 claims description 25
- 239000000463 material Substances 0.000 claims description 23
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 14
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 12
- 239000000706 filtrate Substances 0.000 claims description 12
- 241001165494 Rhodiola Species 0.000 claims description 9
- 239000000047 product Substances 0.000 claims description 9
- 238000003795 desorption Methods 0.000 claims description 8
- 238000010438 heat treatment Methods 0.000 claims description 7
- 238000001179 sorption measurement Methods 0.000 claims description 7
- 239000011229 interlayer Substances 0.000 claims description 5
- 229920000742 Cotton Polymers 0.000 claims description 3
- 239000007788 liquid Substances 0.000 claims description 3
- 238000011049 filling Methods 0.000 claims description 2
- 238000002203 pretreatment Methods 0.000 claims 1
- 238000002360 preparation method Methods 0.000 abstract description 8
- 239000008213 purified water Substances 0.000 description 8
- 238000010586 diagram Methods 0.000 description 4
- 239000002994 raw material Substances 0.000 description 4
- 244000042430 Rhodiola rosea Species 0.000 description 3
- 235000003713 Rhodiola rosea Nutrition 0.000 description 3
- 238000004321 preservation Methods 0.000 description 3
- 230000000694 effects Effects 0.000 description 2
- 239000000284 extract Substances 0.000 description 2
- 238000001556 precipitation Methods 0.000 description 2
- 206010028980 Neoplasm Diseases 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 235000019658 bitter taste Nutrition 0.000 description 1
- 201000011510 cancer Diseases 0.000 description 1
- 230000002526 effect on cardiovascular system Effects 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- 239000003205 fragrance Substances 0.000 description 1
- 230000036039 immunity Effects 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000000874 microwave-assisted extraction Methods 0.000 description 1
- 239000000419 plant extract Substances 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
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Classifications
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07H—SUGARS; DERIVATIVES THEREOF; NUCLEOSIDES; NUCLEOTIDES; NUCLEIC ACIDS
- C07H15/00—Compounds containing hydrocarbon or substituted hydrocarbon radicals directly attached to hetero atoms of saccharide radicals
- C07H15/18—Acyclic radicals, substituted by carbocyclic rings
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07H—SUGARS; DERIVATIVES THEREOF; NUCLEOSIDES; NUCLEOTIDES; NUCLEIC ACIDS
- C07H1/00—Processes for the preparation of sugar derivatives
- C07H1/06—Separation; Purification
- C07H1/08—Separation; Purification from natural products
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Biochemistry (AREA)
- Biotechnology (AREA)
- General Health & Medical Sciences (AREA)
- Genetics & Genomics (AREA)
- Molecular Biology (AREA)
- Extraction Or Liquid Replacement (AREA)
Abstract
The invention aims to provide a preparation method for extracting salidroside, which comprises a preparation method and a device thereof. The salidroside finished product is obtained by utilizing an extraction device for pretreatment and extraction, filtering through a nanofiltration membrane, adsorbing and desorbing through macroporous resin, and finally concentrating and drying. The invention utilizes the product prepared by the special extraction device and the process method, effectively reduces the preparation time of the product, simplifies the operation steps and improves the product purity.
Description
Technical Field
The invention relates to a preparation method of a plant extract, and particularly relates to a method for extracting salidroside.
Background
The rhodiola rosea extract is an extract of the root of rhodiola rosea, and has fragrant and sweet smell and bitter taste. The main component is salidroside, and has effects of enhancing immunity, protecting cardiovascular and cerebrovascular system, and resisting cancer and depression. Chinese patent (application number: CN 2013100149469) discloses a method for separating and purifying salidroside in natural rhodiola rosea: slicing the rhodiola root raw material, performing microwave-assisted extraction, performing alcohol precipitation and concentration, and purifying by extraction and back extraction to finally obtain a finished product. Although the method can prepare salidroside with high purity, the preparation process needs to be kept stand for 24 hours in the alcohol precipitation stage, and the preparation method lasts too long. Chinese patent (application No. CN 2016106114433) discloses a method for preparing salidroside from radix Rhodiolae, which comprises the following steps: slicing rhodiola root raw material, extracting with water, stripping to remove impurities, extracting and back-extracting, crystallizing and purifying to obtain the product. The method slices the raw material, but reduces the contact area of the raw material and the extractant, influences the extraction effect and has low product yield.
Disclosure of Invention
The invention aims to provide a method for extracting salidroside, which effectively reduces the preparation time of products, simplifies the operation steps and improves the purity of the products by a special extraction device.
The scheme adopted by the invention for solving the problems is as follows:
a method for extracting salidroside comprises the following steps:
s1 pretreatment: putting the cleaned rhodiola root into an extraction device for pretreatment, and keeping a certain temperature and pressure;
s2 extraction: smashing rhodiola root by an extraction device, keeping a certain temperature and pressure, extracting by ultrasonic assistance, and stirring to obtain an extracting solution;
s3 filtering: using a nanofiltration membrane for the extracting solution to obtain filtrate;
adsorption and desorption of S4 resin: enabling the filtrate to flow through a resin column, and enabling a desorbent to flow through the resin column to obtain a purified solution;
s5, concentrating the purified solution, and drying to obtain the finished product.
Further, the pretreatment step, setting the temperature of the extraction device at 80-100 ℃ and treating for 30-60 minutes under the condition of 0.1-0.2 Mpa.
Further, the extraction step is that the temperature of the extraction device is set to be 55-75 ℃, the material is broken for 10-30 minutes under the condition of 0.1-0.2Mpa, and the ultrasonic frequency is 20000-25000 Hz.
Further, in the filtering step, the water phase interception molecular weight of the nanofiltration membrane is 350-450.
Further, in the resin adsorption and desorption step, nonpolar macroporous resin is used for filling the resin column, filtrate flows through the resin column at the flow rate of 2.5-3.5BV/h, and 15-30% ethanol is used for desorption at the flow rate of 4-5 BV/h.
More specifically, the non-polar macroporous resin is: ASD-115 or LX-T28.
More specifically, the length-diameter ratio of the resin column is 1-1.5: 50.
More specifically, adopt extraction element to carry out preliminary treatment and extraction, wherein extraction element includes aircraft nose 1 and jar body 2, its characterized in that: a motor 3 is arranged in the machine head 1, the motor 3 is connected with a stirring device 4, and the outer surface of a projecting part 1-1 at the lower end of the machine head 1 is provided with threads and is in threaded connection with a material bin 5; the inner surface of the bottom of the tank body 2 is provided with a heating device 6, the center of the bottom of the tank body 2 is provided with a stirring paddle 8, the bottom of the tank body 2 is provided with an ultrasonic generating device 7, and the upper part of the tank body is provided with a pressure control device 9 close to the machine head 1.
Furthermore, the side wall and the bottom of the material bin 5 are provided with 80-120 meshes for preventing the material from flowing out of the material bin 5 and separating the material liquid.
Further, 2 lateral walls of the tank body are provided with heat preservation interlayers, and heat preservation cotton is filled in the interlayers.
The beneficial effect of this scheme: (1) the preparation time is effectively shortened by using a unique extraction device; (2) the product yield is improved, and the cost is reduced; (3) the purity of the product is effectively improved by using special macroporous resin purification parameters.
Drawings
The accompanying drawings are not intended to be drawn to scale, and wherein: fig. 1 is an overall structural diagram of the extraction device, fig. 2 is a structural diagram of a head of the extraction device, fig. 3 is a structural diagram of a tank body of the extraction device, and fig. 4 is a schematic diagram of a material bin of the extraction device.
Wherein the indices represent the following meanings: 1-machine head, 1-1 projecting part, 2-tank body, 3-motor, 4-stirring device, 5-material bin, 6-heating device, 7-ultrasonic generating device, 8-stirring paddle and 9-pressure control device.
Detailed Description
Example 1
Cutting 1kg radix Rhodiolae into small segments, placing into a material bin of an extraction device, adding 4.5L purified water, setting the temperature of the extraction device at 80 deg.C and the internal pressure at 0.1 Mpa. In the pretreatment process, the stirring device and the ultrasonic generating device of the extraction device do not work, the heating device heats the purified water, and the pressure control device releases the pressure to keep the set pressure when the steam reaches the set pressure because the tank body is sealed. After pretreatment for 60min, the stirring device is started, the material is cut up for 10min, and simultaneously, the temperature is set to 60 ℃, the internal pressure is set to 0.1Mpa, and the ultrasonic frequency is 20000Hz for extraction. In the extraction process, when the stirring device stops cutting the materials, the stirring paddle starts to work, the ultrasonic generating device starts to work at the same time, and the extraction is carried out for 60min under the conditions to obtain the extracting solution. Filtering the extractive solution with nanofiltration membrane with water phase molecular weight cutoff of 350 to obtain filtrate. The filtrate was passed through a resin column having a diameter of 2cm and a length of 50cm, and the resin column was packed with ASD-115 at an adsorption rate of 2.5 BV/h. Using 15 percent ethanol, and obtaining the analysis solution at the desorption rate of 4 BV/h. The eluate was concentrated and dried to obtain 8.43g of salidroside with a yield of 85.4%.
Example 2
Cutting 1.5kg radix Rhodiolae into small segments, placing into a material bin of an extraction device, adding 7L purified water, setting the temperature of the extraction device at 100 deg.C and the internal pressure at 0.2 Mpa. In the pretreatment process, the stirring device and the ultrasonic generating device of the extraction device do not work, the heating device heats the purified water, and the pressure control device releases the pressure to keep the set pressure when the steam reaches the set pressure because the tank body is sealed. After 30min of pretreatment, the stirring device was turned on, and the material was chopped for 15min while the temperature was set at 90 ℃, the internal pressure at 0.2Mpa, and the ultrasonic frequency at 25000Hz for extraction. In the extraction process, when the stirring device stops cutting the materials, the stirring paddle starts to work, the ultrasonic generating device starts to work at the same time, and extraction is carried out for 30min under the conditions to obtain the extracting solution. Filtering the extractive solution with nanofiltration membrane with water phase molecular weight cutoff of 450 to obtain filtrate. The filtrate was passed through a resin column having a diameter of 4cm and a length of 50cm, and the resin column was packed with LX-T28 at an adsorption rate of 3.5 BV/h. Using 30 percent ethanol, and obtaining the analysis solution with the desorption rate of 5 BV/h. The eluate was concentrated and dried to obtain 13.27g of salidroside with a yield of 86.1%.
Example 3
Cutting 1.2kg radix Rhodiolae into small segments, placing into a material bin of an extraction device, adding 5L purified water, setting the temperature of the extraction device at 95 deg.C and the internal pressure at 0.18 Mpa. In the pretreatment process, the stirring device and the ultrasonic generating device of the extraction device do not work, the heating device heats the purified water, and the pressure control device releases the pressure to keep the set pressure when the steam reaches the set pressure because the tank body is sealed. After 50min of pretreatment, the stirring device is started, the materials are cut up for 30min, and simultaneously, the temperature is set to 80 ℃, the internal pressure is set to 0.2Mpa, and the ultrasonic frequency is 23000Hz for extraction. In the extraction process, when the stirring device stops cutting the materials, the stirring paddle starts to work, the ultrasonic generating device starts to work at the same time, and the extraction is carried out for 60min under the conditions to obtain the extracting solution. Filtering the extractive solution with nanofiltration membrane with water phase molecular weight cutoff of 400 to obtain filtrate. The filtrate was passed through a resin column having a diameter of 3cm and a length of 50cm, and the resin column was packed with LX-T28 at an adsorption rate of 3 BV/h. Using 20 percent ethanol, and obtaining the analysis solution with the desorption rate of 4.5 BV/h. The eluate was concentrated and dried to obtain 9.83g of salidroside with a yield of 82.1%.
Example 4
The rhodiola root is cut into small sections and put into a material bin of an extraction device, and the material bin is fixed at the protruding part of the machine head through threads. Adding purified water, and setting the temperature and pressure of pretreatment. In the pretreatment process, the stirring device and the ultrasonic generating device of the extraction device do not work, the heating device heats the purified water, and the pressure control device releases the pressure to keep the set pressure when the steam reaches the set pressure because the tank body is sealed. After the pretreatment is finished, the extraction temperature and the pressure are reset, the stirring device is started, and the motor rotates to drive the stirring device to shred the rhodiola roots. The side wall and the bottom of the bin are provided with sieve pores, so that the rhodiola root can be ensured not to be diffused into liquid while being cut. In the extraction process, when the stirring device stops cutting the materials, the stirring paddle starts to work, and the ultrasonic generating device starts to work at the same time. Because the tank body of the extraction device is sealed and the interlayer is provided with the heat preservation cotton, certain temperature and pressure can be maintained, and finally the extracting solution is obtained.
Claims (10)
1. A method for extracting salidroside comprises the following steps:
s1 pretreatment: putting the cleaned rhodiola root into an extraction device for pretreatment, and keeping a certain temperature and pressure;
s2 extraction: smashing the pretreated rhodiola root by an extraction device, keeping a certain temperature and pressure, extracting by ultrasonic assistance, and stirring to obtain an extracting solution;
s3 filtering: filtering the extractive solution with nanofiltration membrane to obtain filtrate;
adsorption and desorption of S4 resin: enabling the filtrate to flow through a resin column, and enabling a desorbent to flow through the resin column to obtain a purified liquid;
s5, concentrating the purified solution, and drying to obtain the finished product.
2. The method according to claim 1, wherein the pre-treating step comprises treating the extraction device at 80-100 deg.C and 0.1-0.2MPa for 30-60 min.
3. The method for extracting salidroside as claimed in claim 1, wherein said extracting step comprises breaking the material at 60-90 deg.C under 0.1-0.2MPa for 10-30 min with 20000-25000Hz ultrasonic frequency.
4. The method as claimed in claim 1, wherein the nanofiltration membrane has a water phase molecular weight cut-off of 350-450.
5. The method of claim 1, wherein the resin adsorption and desorption step comprises filling a resin column with nonpolar macroporous resin, passing the filtrate through the resin column at a flow rate of 2.5-3.5BV/h, and desorbing with 15-30% ethanol at a flow rate of 4-5 BV/h.
6. The method for extracting salidroside according to claim 5, wherein said non-polar macroporous resin is: ASD-115 or LX-T28.
7. The method for extracting salidroside according to claim 5, wherein said resin column length to diameter ratio is 2-4: 50.
8. The method for extracting salidroside according to any of claims 1-7, wherein an extraction device is used for pre-treatment and extraction; the extraction device comprises a machine head (1) and a tank body (2), a motor (3) is arranged in the machine head (1), the motor (3) is connected with a stirring device (4), and the outer surface of a protruding part (1-1) at the lower end of the machine head (1) is provided with threads and is in threaded connection with a material bin (5); the inner surface of the bottom of the tank body (2) is provided with a heating device (6), the center of the bottom of the tank body (2) is provided with a stirring paddle (8), the bottom of the tank body (2) is provided with an ultrasonic generating device (8), and the upper part of the tank body is provided with a pressure control device (9) close to the machine head (1).
9. The method for extracting salidroside according to claim 8, wherein said side walls and bottom of said material bin (5) are provided with 80-120 mesh sieve holes.
10. The method for extracting salidroside according to claim 8, wherein the side wall of said tank (2) is provided with a heat-insulating interlayer, and the interlayer is filled with heat-insulating cotton.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202110921820.4A CN113603734A (en) | 2021-08-12 | 2021-08-12 | Method for extracting salidroside |
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| Application Number | Priority Date | Filing Date | Title |
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| CN202110921820.4A CN113603734A (en) | 2021-08-12 | 2021-08-12 | Method for extracting salidroside |
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| CN113603734A true CN113603734A (en) | 2021-11-05 |
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Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1880326A (en) * | 2005-06-16 | 2006-12-20 | 周晓明 | Two-step resin method for preparing salidrose |
| CN103467540A (en) * | 2013-10-09 | 2013-12-25 | 白心亮 | Method for extracting salidroside from rhodiola |
| CN106432379A (en) * | 2016-10-21 | 2017-02-22 | 乌鲁木齐上善元生物科技有限公司 | Method for extracting salidroside from rhodiola |
| CN108095117A (en) * | 2018-01-02 | 2018-06-01 | 广州泽力医药科技有限公司 | Gadol extract and its extracting method and application |
| CN210278330U (en) * | 2019-07-18 | 2020-04-10 | 伯特瑞(福建)生物科技有限公司 | Multifunctional dynamic separation and extraction device for active ingredients of mushrooms |
| CN211025210U (en) * | 2019-08-09 | 2020-07-17 | 张瑞麟 | Plant extraction equipment of daily use chemicals production usefulness |
| CN112403023A (en) * | 2020-11-16 | 2021-02-26 | 云南滇药医药健康产业有限公司 | Equipment and method for extracting effective components of traditional Chinese medicine |
-
2021
- 2021-08-12 CN CN202110921820.4A patent/CN113603734A/en active Pending
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1880326A (en) * | 2005-06-16 | 2006-12-20 | 周晓明 | Two-step resin method for preparing salidrose |
| CN103467540A (en) * | 2013-10-09 | 2013-12-25 | 白心亮 | Method for extracting salidroside from rhodiola |
| CN106432379A (en) * | 2016-10-21 | 2017-02-22 | 乌鲁木齐上善元生物科技有限公司 | Method for extracting salidroside from rhodiola |
| CN108095117A (en) * | 2018-01-02 | 2018-06-01 | 广州泽力医药科技有限公司 | Gadol extract and its extracting method and application |
| CN210278330U (en) * | 2019-07-18 | 2020-04-10 | 伯特瑞(福建)生物科技有限公司 | Multifunctional dynamic separation and extraction device for active ingredients of mushrooms |
| CN211025210U (en) * | 2019-08-09 | 2020-07-17 | 张瑞麟 | Plant extraction equipment of daily use chemicals production usefulness |
| CN112403023A (en) * | 2020-11-16 | 2021-02-26 | 云南滇药医药健康产业有限公司 | Equipment and method for extracting effective components of traditional Chinese medicine |
Non-Patent Citations (1)
| Title |
|---|
| 张俊庭主编: "中国中医药最新研创大全", 北京：中医古籍出版社, pages: 2119 - 2121 * |
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Application publication date: 20211105 |