CN113121715A - A method for separating and extracting rhizoma Polygonati polysaccharide with intestinal mucosa immunocompetence - Google Patents
A method for separating and extracting rhizoma Polygonati polysaccharide with intestinal mucosa immunocompetence Download PDFInfo
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- 150000004676 glycans Chemical class 0.000 title claims abstract description 45
- 229920001282 polysaccharide Polymers 0.000 title claims abstract description 45
- 239000005017 polysaccharide Substances 0.000 title claims abstract description 45
- 238000000034 method Methods 0.000 title claims abstract description 41
- 210000004347 intestinal mucosa Anatomy 0.000 title claims abstract description 19
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 63
- 241000756042 Polygonatum Species 0.000 claims abstract description 48
- 239000002245 particle Substances 0.000 claims abstract description 30
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 19
- 239000012153 distilled water Substances 0.000 claims abstract description 18
- 238000002791 soaking Methods 0.000 claims abstract description 10
- 239000006228 supernatant Substances 0.000 claims abstract description 10
- 238000002137 ultrasound extraction Methods 0.000 claims abstract description 7
- 238000002386 leaching Methods 0.000 claims abstract description 6
- 238000005406 washing Methods 0.000 claims abstract description 6
- 238000001035 drying Methods 0.000 claims abstract description 5
- 238000002156 mixing Methods 0.000 claims abstract description 5
- 239000002244 precipitate Substances 0.000 claims abstract description 5
- 238000001291 vacuum drying Methods 0.000 claims abstract description 5
- 239000012530 fluid Substances 0.000 claims abstract description 4
- 230000001376 precipitating effect Effects 0.000 claims abstract description 3
- 238000010438 heat treatment Methods 0.000 claims description 18
- 239000007921 spray Substances 0.000 claims description 15
- 239000002904 solvent Substances 0.000 claims description 10
- 238000007789 sealing Methods 0.000 claims description 8
- 238000001816 cooling Methods 0.000 claims description 7
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- 239000002028 Biomass Substances 0.000 abstract description 2
- 238000001556 precipitation Methods 0.000 description 7
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- 241000894006 Bacteria Species 0.000 description 1
- 206010061218 Inflammation Diseases 0.000 description 1
- 241000234280 Liliaceae Species 0.000 description 1
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- 230000032683 aging Effects 0.000 description 1
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08B—POLYSACCHARIDES; DERIVATIVES THEREOF
- C08B37/00—Preparation of polysaccharides not provided for in groups C08B1/00 - C08B35/00; Derivatives thereof
- C08B37/0003—General processes for their isolation or fractionation, e.g. purification or extraction from biomass
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- Materials Engineering (AREA)
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Abstract
The invention discloses a method for separating and extracting polygonatum polysaccharide with intestinal mucosa immunocompetence, belonging to the technical field of biomass extraction, comprising the following steps: s1: preparing 2-3 cm rhizoma polygonati slices, drying the rhizoma polygonati slices, crushing the rhizoma polygonati slices into rhizoma polygonati particles with the particle size of 0.1-0.15 mm by using supersonic speed crushing equipment, and placing the particles in a container for later use; s2: adding distilled water into a container, and soaking for 1-2 days to obtain a first sealwort solution and residues; s3: adding distilled water into the residue, leaching for 20-30 min at 73-85 ℃, and performing ultrasonic extraction for 15-25 min to obtain a second rhizoma polygonati solution; s4: mixing the first rhizoma polygonati solution and the second rhizoma polygonati solution to form a third rhizoma polygonati solution, centrifuging the third rhizoma polygonati solution, and taking supernatant fluid of the third rhizoma polygonati solution; s5: adding the first ethanol solution into the supernatant, precipitating with ethanol, standing, centrifuging, collecting precipitate, washing with the second ethanol solution, and vacuum drying to obtain rhizoma Polygonati polysaccharide. The method is simple, and can improve the yield of rhizoma Polygonati polysaccharide.
Description
Technical Field
The invention belongs to the technical field of biomass extraction, and particularly relates to a separation and extraction method of polygonatum polysaccharide with intestinal mucosa immunocompetence.
Background
Rhizoma Polygonati is dried rhizome of Polygonatum sibiricum Red, Polygonatum kingianum, Polygonatum sibiricum Rehd, etc. of Liliaceae, and is a special plant in Shaoyong city of Shaoyang city in Hunan province, also called rhizoma Polygonati and radix Caraganae Sinicae. It has effects of invigorating spleen, replenishing qi, nourishing heart and lung, strengthening tendons and bones, and prolonging life after long-term administration, and is a plant with homology of medicine and food. Modern pharmacological research shows that the main chemical components in the sealwort are as follows: rhizoma Polygonati polysaccharide.
Pharmacological research proves that the polygonatum polysaccharide participates in various activities of cells and organisms in life phenomena, and has the effects of resisting oxidation, aging, tumors and atherosclerosis, inhibiting bacteria, resisting inflammation, resisting fatigue, reducing blood sugar, blood fat, improving intestinal mucosa immunocompetence and the like.
At present, the extraction of polygonatum polysaccharide mainly comprises a water extraction method, an ultrasonic wave, microwave auxiliary extraction method and other methods, the separation and refinement mainly comprises the traditional water extraction and alcohol precipitation method, macroporous resin adsorption, membrane separation and other methods and coupling among different methods, in the prior art, polygonatum polysaccharide is generally extracted by using polygonatum particles or polygonatum slices, the yield of polygonatum polysaccharide can reach 48%, researches show that the dissolution rate of traditional Chinese medicinal materials is influenced by the particle size, and in the extraction methods, the extraction amount of polygonatum polysaccharide is less due to the adoption of raw materials with larger particle size.
Disclosure of Invention
In order to solve the above problems, the present invention aims to provide a method for separating and extracting polygonatum polysaccharide with intestinal mucosa immunocompetence, so as to increase the yield of polygonatum polysaccharide.
In order to achieve the purpose, the technical scheme of the invention is as follows: a method for separating and extracting rhizoma Polygonati polysaccharide with intestinal mucosa immunocompetence comprises the following steps:
s1: preparing 2-3 cm rhizoma polygonati slices, drying the rhizoma polygonati slices, crushing the rhizoma polygonati slices into rhizoma polygonati particles with the particle size of 0.1-0.15 mm by using supersonic speed crushing equipment, and placing the particles in a container for later use;
s2: adding distilled water into a container, and soaking for 1-2 days to obtain a first sealwort solution and residues;
s3: adding distilled water into the residue, leaching for 20-30 min at 73-85 ℃, and then performing ultrasonic extraction for 15-25 min to obtain a second sperm solution;
s4: mixing the first rhizoma polygonati solution and the second rhizoma polygonati solution to form a third rhizoma polygonati solution, centrifuging the third rhizoma polygonati solution, and taking supernatant fluid of the third rhizoma polygonati solution;
s5: adding the first ethanol solution into the supernatant, precipitating with ethanol, standing, centrifuging, collecting precipitate, washing with the second ethanol solution, and vacuum drying to obtain rhizoma Polygonati polysaccharide.
Further, in S2, the soaking method includes the following steps: the method comprises the following steps: heating rhizoma Polygonati granules and distilled water; step two: and obtaining a first sealwort solution every 3-4 hours, and filtering the obtained first sealwort solution.
Further, in the first step, the heating temperature is as follows: 41-55 ℃.
Further, in the second step, the obtained first rhizoma polygonati solution is filtered by using a 170-mesh screen.
Further, in S4, the third rhizoma Polygonati solution is filtered through a 170-200 mesh screen.
Further, in S5, the first ethanol solution is 60 vol% to 95 vol% ethanol.
Further, in S5, the second ethanol solution is 95 vol% ethanol.
Further, the container comprises a rack and an outer barrel fixed on the rack, wherein the outer barrel is internally provided with an inner barrel with an upper opening, the inner barrel is rotatably connected with a cover plate for sealing the opening, a driving piece is fixed on the rack, an output shaft of the driving piece is fixedly connected with the cover plate, a solvent spray head and a gas spray head are fixed on the cover plate, a first screen is arranged on the side wall of the inner barrel, and a baffle plate for sealing the first screen is vertically and slidably connected on the cover plate; the bottom of the outer cylinder is provided with a second screen, the inner cylinder is fixed with a pneumatic piece, and an output shaft of the pneumatic piece is fixed with a sealing plate for sealing the second screen.
Further, a liquid inlet spray head and a recoverer are fixed on the outer cylinder.
Furthermore, the recoverer comprises a body, a collecting cavity is formed in the body, the collecting cavity is communicated with an air inlet one-way valve fixed on the body, a cooling cavity is formed in the body, and a cold source is arranged in the cooling cavity.
After the scheme is adopted, the following beneficial effects are realized: (1) in S1 and S2, the sealwort is sliced and crushed into sealwort particles with supersonic speed, the particle size is 0.1 mm-0.15 mm, so as to improve the dissolution rate of the sealwort, the dissolution rate of the polygonatum polysaccharide is improved when the sealwort particles are soaked, and the dissolution rate of the polygonatum polysaccharide is further improved by heating during soaking, so that the yield of the polygonatum polysaccharide is improved.
(2) In S3, S4 and S5, because part of polygonatum polysaccharide still remains in the residues after soaking, the residual polygonatum polysaccharide is extracted by utilizing leaching and ultrasonic extraction, the yield of the polygonatum polysaccharide is improved, and polygonatum polysaccharide particles with higher purity are obtained by utilizing alcohol precipitation, standing, centrifugation and washing.
(3) In the scheme, the polygonatum particles are soaked, the temperature is 41-55 ℃, the residues are extracted at the temperature of 73-85 ℃, so that the time for the residues to reach 73-85 ℃ from 41-55 ℃ is short, energy is saved compared with the process of heating from room temperature to 73-85 ℃, and the extraction cost of polygonatum polysaccharide is reduced to a certain extent.
Drawings
FIG. 1 is a schematic view of a container according to a second embodiment of the present invention;
fig. 2 is a schematic diagram of a recoverer according to a second embodiment of the present invention.
Detailed Description
The following is further detailed by way of specific embodiments:
reference numerals in the drawings of the specification include: the device comprises an outer cylinder 11, a cavity 12, a recoverer 13, an air inlet one-way valve 131, a cooling cavity 132, a collecting cavity 134, a cover plate 14, a feeding spray head 15, a motor 16, a first solvent spray head 17, an inner cylinder 18, a second solvent spray head 19, a first screen 20, a baffle plate 21, an air cylinder 22, a heating device 23, a closing plate 24, a collecting box 25, a second screen 26 and an ultrasonic generator 27.
The first embodiment is as follows:
a method for separating and extracting rhizoma Polygonati polysaccharide with intestinal mucosa immunocompetence comprises the following steps:
s1: preparing 2-3 cm rhizoma polygonati slices, drying the rhizoma polygonati slices, crushing the rhizoma polygonati slices into rhizoma polygonati particles with the particle size of 0.1-0.15 mm by using supersonic speed crushing equipment, and placing the particles in a container for later use;
s2: adding distilled water into a container, wherein the mass ratio of the polygonatum particles to the distilled water is 1: 6-1: 8, for example, 12kg of distilled water is needed for 1kg of polygonatum particles, and soaking the polygonatum particles for 1-2 days, wherein the soaking mode comprises the following steps: step one, heating rhizoma polygonati particles and distilled water at the temperature of 41-55 ℃; step two: obtaining a first sealwort solution every 3-4 hours, finally obtaining the first sealwort solution and residues, and filtering the obtained first sealwort solution by using a 170-mesh screen;
s3: adding distilled water into the residue, leaching for 20-30 min at 73-85 ℃, and then performing ultrasonic extraction for 15-25 min to obtain a second sperm solution;
s4: mixing the first rhizoma polygonati solution and the second rhizoma polygonati solution to form a third rhizoma polygonati solution, filtering the third rhizoma polygonati solution by using a screen mesh of 170-200 meshes, centrifuging the third rhizoma polygonati solution, and taking supernatant fluid;
s5: adding a first ethanol solution into the supernate to carry out alcohol precipitation, standing the first ethanol solution with 60-95 vol% ethanol, centrifuging, taking precipitate, washing with a second ethanol solution with 95 vol% ethanol, and carrying out vacuum drying to obtain the polygonatum polysaccharide.
In the embodiment, the polygonatum particles are extracted, so that the dissolution rate of polygonatum polysaccharide is improved, the polygonatum is extracted, then the residues are extracted and subjected to ultrasonic extraction, the polygonatum polysaccharide is extracted from the polygonatum to the maximum extent, and the extraction amount of the polygonatum polysaccharide is improved. And secondly, multiple times of filtration are carried out, so that the impurities of the polygonatum sibiricum are reduced, and the purity of the polygonatum sibiricum polysaccharide is improved.
Example two:
a method for separating and extracting rhizoma Polygonati polysaccharide with intestinal mucosa immunocompetence comprises the following steps: s1: preparing 2 cm-3 cm rhizoma Polygonati slices, drying the rhizoma Polygonati slices, pulverizing the rhizoma Polygonati slices into rhizoma Polygonati particles of 0.1 mm-0.15 mm by supersonic pulverizing equipment, and placing in an inner cylinder 18 of a container as shown in figures 1 and 2, wherein in this embodiment, the container comprises a frame, an outer cylinder 11 is fixed on the frame by bolts, the inner cylinder 18 is rotatably connected with the frame and arranged in the outer cylinder 11, a cavity 12 is formed between the inner cylinder 18 and the outer cylinder 11, the inner cylinder 18 is hollow and has an opening at the upper part, a cover plate 14 is arranged on the inner cylinder 18, one side of the cover plate 14 is rotatably connected with the inner cylinder 18, the other side of the cover plate 14 is detachably connected with the inner cylinder 18, the frame is provided with a driving part, in this embodiment, the driving part is a motor 16, an output shaft of the motor 16 is fixedly connected with the cover plate 14, a first solvent spray nozzle 17 and a feeding spray nozzle 15 are fixed on, a heating device 23 is fixed on the bolt in the side wall of the inner cylinder 18, such as: the heating coil, the first screen cloth 20 of 170 mesh is fixed on the lateral wall of inner tube 18 with the screw, connect with the baffle 21 used for closing the first screen cloth 20 on the vertical sliding connection of apron 14.
The bottom of the outer cylinder 11 is conical, a second screen 26 with a 170-200 mesh sieve is fixed on the bottom of the outer cylinder 11 through screws, an air cylinder 22 is fixed on the inner cylinder 18, a closing plate 24 for closing the second screen 26 is fixed on an output shaft of the air cylinder 22, a heater is installed on the side wall of the outer cylinder 11, and a collecting box 25 is arranged below the outer cylinder 11. The outer barrel 11 is fixed with a second solvent spray nozzle 19 and a recoverer 13, as shown in fig. 2, the recoverer 13 includes a body, a collection chamber 134 is formed in the body, the collection chamber 134 is communicated with an air inlet check valve 131, the air inlet check valve 131 is fixed on the body, a cooling chamber 132 is formed on the side wall of the body, and a cold source is installed in the cooling chamber 132, wherein the cold source is ice cubes in the embodiment.
S2: in the embodiment, polygonatum particles are sprayed into the inner cylinder 18 through the feeding spray nozzle 15, meanwhile, distilled water is sprayed into the inner cylinder 18 through the first solvent spray nozzle 17, so that the purpose of fully mixing the distilled water with the polygonatum particles is achieved, the polygonatum particles are soaked in the distilled water for 1-2 d, the heating device 23 is started in the soaking process, the heating device 23 heats the polygonatum particles, the heating temperature reaches 41-55 ℃, the baffle 21 is taken away every 3-4 h, the motor 16 is started, the motor 16 drives the cover plate 14 and the inner cylinder 18 to rotate, a first polygonatum solution is centrifugally extracted for 2-5 min every time, and distilled water is supplemented into the inner cylinder 18 after the first polygonatum solution is extracted. The first sealwort solution is filtered by the first screen 20 under the centrifugal action and then enters the cavity 12 for storage.
S3: after the first sealwort solution is extracted for a plurality of times, the first screen 20 is sealed by the baffle 21, distilled water is added through the first solvent spray nozzle 17, the temperature of the heating device 23 is controlled to be 73-85 ℃, the leaching is carried out for 20-30 min at the temperature of 73-85 ℃, then the ultrasonic generator 27 is started, the residue is subjected to ultrasonic extraction for 15-25 min, and a second sealwort solution is obtained. The baffle 21 is removed, the motor 16 is started, the motor 16 drives the inner barrel 18 to rotate, and the second sperm solution enters the cavity 12 through the first screen 20 under the centrifugal action.
S4: the first sealwort solution and the second sealwort solution entering the cavity 12 are mixed to form a third sealwort solution, the cylinder 22 is started, the cylinder 22 drives the closing plate 24, the second screen 26 is opened by the closing plate 24, and the third sealwort is dissolved and enters the collection box 25 through the second screen 26. And placing the collection box 25 in the inner cylinder 18 and fixing, starting the motor 16 again, driving the inner cylinder 18 and the collection box 25 to rotate by the motor 16, thus carrying out centrifugal operation on the third sealwort solution, and taking supernatant liquid by an operator through a needle cylinder.
S5: after the centrifugal separation is completed, the supernatant is sent into the cavity 12 through the second solvent nozzle 19 (at this time, the cylinder 22 drives the closing plate 24 to close the second screen 26), and the supernatant is sent into the 60-95 vol% first ethanol solution through the second solvent nozzle 19 for alcohol precipitation. Then, a closing plate 24 is driven by an air cylinder 22, the solution after alcohol precipitation is filtered by a second screen 26 and collected in a collection box 25, standing is carried out again, the precipitate is taken out, and then 95 vol% of second ethanol solution is used for washing and vacuum drying, so that the polygonatum polysaccharide is obtained. In the alcohol precipitation process, the atmospheric pressure in the collection chamber 134 can become low to the low temperature of ice-cube, and atmospheric pressure in the cavity 12 is higher (owing to the heating effect), and under atmospheric pressure's effect, volatile ethanol can enter into collection chamber 134 through admitting air check valve 131 in order to reach the purpose of retrieving ethanol.
In this embodiment, the container is suitable for the reuse of a plurality of steps, has reduced the transfer of operating personnel's equipment in the polygonatum polysaccharide extraction process, has improved the extraction efficiency of polygonatum polysaccharide to a certain extent promptly. Meanwhile, the heating device is used for continuously heating the residues in the scheme, so that S3 and S4 are more continuous, and the heating energy consumption is reduced. In the scheme, in the alcohol precipitation process, ethanol is recycled for secondary utilization, so that certain ethanol cost is reduced.
The foregoing is merely an example of the present invention and common general knowledge in the art of specific structures and/or features of the invention has not been set forth herein in any way. It should be noted that, for those skilled in the art, without departing from the structure of the present invention, several changes and modifications can be made, which should also be regarded as the protection scope of the present invention, and these will not affect the effect of the implementation of the present invention and the practicability of the patent. The scope of the claims of the present application shall be determined by the contents of the claims, and the description of the embodiments and the like in the specification shall be used to explain the contents of the claims.
Claims (10)
1. A method for separating and extracting rhizoma polygonati polysaccharide with intestinal mucosa immunocompetence is characterized by comprising the following steps: the method comprises the following steps:
s1: preparing 2-3 cm rhizoma polygonati slices, drying the rhizoma polygonati slices, crushing the rhizoma polygonati slices into rhizoma polygonati particles with the particle size of 0.1-0.15 mm by using supersonic speed crushing equipment, and placing the particles in a container for later use;
s2: adding distilled water into a container, and soaking for 1-2 days to obtain a first sealwort solution and residues;
s3: adding distilled water into the residue, leaching for 20-30 min at 73-85 ℃, and then performing ultrasonic extraction for 15-25 min to obtain a second sperm solution;
s4: mixing the first rhizoma polygonati solution and the second rhizoma polygonati solution to form a third rhizoma polygonati solution, centrifuging the third rhizoma polygonati solution, and taking supernatant fluid of the third rhizoma polygonati solution;
s5: adding the first ethanol solution into the supernatant, precipitating with ethanol, standing, centrifuging, collecting precipitate, washing with the second ethanol solution, and vacuum drying to obtain rhizoma Polygonati polysaccharide.
2. The method for separating and extracting polygonatum polysaccharides with intestinal mucosa immunocompetence according to claim 1, wherein the method comprises the following steps: in S2, the soaking method includes the following steps:
the method comprises the following steps: heating rhizoma Polygonati granules and distilled water;
step two: and obtaining a first sealwort solution every 3-4 hours, and filtering the obtained first sealwort solution.
3. The method for separating and extracting polygonatum polysaccharides with intestinal mucosa immunocompetence according to claim 2, wherein the method comprises the following steps: in the first step, the heating temperature is as follows: 41-55 ℃.
4. The method for separating and extracting polygonatum polysaccharides with intestinal mucosa immunocompetence according to claim 3, wherein the method comprises the following steps: in the second step, the obtained first sealwort solution is filtered by using a 170-mesh screen.
5. The method for separating and extracting polygonatum polysaccharides with intestinal mucosa immunocompetence according to claim 4, wherein the method comprises the following steps: in S4, filtering the third rhizoma Polygonati solution with a 170-200 mesh screen.
6. The method for separating and extracting polygonatum polysaccharides with intestinal mucosa immunocompetence according to any one of claims 1 to 5, wherein the method comprises the following steps: in S5, the first ethanol solution is 60 vol% to 95 vol% ethanol.
7. The method for separating and extracting polygonatum polysaccharides with intestinal mucosa immunocompetence according to claim 6, wherein the method comprises the following steps: in S5, the second ethanol solution is 95 vol% ethanol.
8. The method for separating and extracting polygonatum polysaccharides with intestinal mucosa immunocompetence according to claim 7, wherein the method comprises the following steps: the container comprises a rack and an outer barrel fixed on the rack, wherein an inner barrel with an opening at the upper part is arranged in the outer barrel, a cover plate for sealing the opening is rotatably connected to the inner barrel, a driving piece is fixed on the rack, an output shaft of the driving piece is fixedly connected with the cover plate, a solvent spray head and a gas spray head are fixed on the cover plate, a first screen is arranged on the side wall of the inner barrel, and a baffle plate for sealing the first screen is vertically and slidably connected to the cover plate; the bottom of the outer cylinder is provided with a second screen, the inner cylinder is fixed with a pneumatic piece, and an output shaft of the pneumatic piece is fixed with a sealing plate for sealing the second screen.
9. The method for separating and extracting polygonatum polysaccharides with intestinal mucosa immunocompetence according to claim 8, wherein the method comprises the following steps: the outer cylinder is fixed with a liquid inlet spray head and a recoverer.
10. The method for separating and extracting polygonatum polysaccharides with intestinal mucosa immunocompetence according to claim 9, wherein the method comprises the following steps: the recoverer comprises a body, a collecting cavity is formed in the body, the collecting cavity is communicated with an air inlet one-way valve fixed on the body, a cooling cavity is formed in the body, and a cold source is arranged in the cooling cavity.
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| CN113817079A (en) * | 2021-11-11 | 2021-12-21 | 云南恩润生物科技发展有限公司 | Extraction method of polygonatum polysaccharide |
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Application publication date: 20210716 |