CN118165132A - Preparation method of low-chroma alcohol-soluble fructus amomi polysaccharide extract - Google Patents
Preparation method of low-chroma alcohol-soluble fructus amomi polysaccharide extract Download PDFInfo
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Landscapes
- Polysaccharides And Polysaccharide Derivatives (AREA)
Abstract
The invention discloses a preparation method of low-chroma alcohol-soluble fructus amomi polysaccharide extract, which comprises the steps of crushing, degreasing, thermal reflux circulation extraction, acidolysis, anti-solvent precipitation, resin separation, pH adjustment, alcohol precipitation, filter pressing, freeze drying and low-temperature crushing of fructus amomi medicinal materials to obtain the low-chroma alcohol-soluble fructus amomi polysaccharide extract. The invention has the advantages of wide sources of raw materials, simple and green preparation process, low chromaticity, high stability and good alcohol solubility of the obtained fructus amomi polysaccharide extract, and is suitable for large-scale production and application.
Description
Technical Field
The invention relates to the technical field of separation and purification of active ingredients of traditional Chinese medicinal materials, in particular to a preparation method of a low-color alcohol-soluble fructus amomi polysaccharide extract.
Background
Fructus Amomi polysaccharide is obtained by extracting fructus Amomi (Amomum villosum Lour.) with solvent, and precipitating with ethanol to obtain extract. Modern researches have proved that fructus Amomi polysaccharide has various activities of improving immunity, regulating lymphocyte, relieving pain and inflammation, and has become a research hotspot in the fields of food, medicine and biology, and has wide application prospect.
The polysaccharide alcohol precipitation technology is a method for separating polysaccharide by reducing the dielectric constant of an aqueous solution to dehydrate polysaccharide, thereby generating precipitation, and is the simplest, quick and easy-to-operate polysaccharide separation method.
The intermittent filter pressing technology is a method of physical compression, under the action of pressure difference, fluid in suspension permeates permeable medium, and solid particles are trapped by the medium, so that the process of separating the fluid from the solid is realized.
The chemical plant degreasing technology is a process for removing lipid in plants by using a chemical method, and uses organic solvents such as ethers, esters, alcohols and the like to extract the plants, and then desolventizes the extract to obtain degreased plant samples.
The alcohol precipitation method is a common method for preparing crude polysaccharide, is simple and quick to operate, is safe and green in production process, and is widely applied to the preparation of all plant polysaccharide; however, the alcohol precipitation method has a large limitation, and the fructus amomi polysaccharide extract directly produced by the alcohol precipitation method has a large amount of plant pigment due to a deep color, and has a large influence on the sensory quality of food after being added, so that decolorization treatment is needed. For example, CN201610350733.7 discloses a method for extracting volatile oil, flavone and polysaccharide from fructus Amomi, the process of preparing fructus Amomi polysaccharide is simple and easy to operate, but the obtained fructus Amomi polysaccharide extract is brown yellow powder, has deep color and poor alcohol solubility, and limits the application range.
The common polysaccharide decoloring method comprises an active carbon adsorption method, a hydrogen peroxide oxidation method, a resin adsorption method and the like, wherein the active carbon treatment time is long, the polysaccharide can be adsorbed, the polysaccharide loss is caused, the particle size of the active carbon is small, and the active carbon is easy to remain in feed liquid and is difficult to remove cleanly or has high removal cost; the oxidation strength of the hydrogen peroxide oxidation method is high, so that polysaccharide hydrolysis is easy to cause, the biological activity is reduced, and the method is not suitable for processing and utilizing food-grade polysaccharide; the resin adsorption method has large specific surface area, strong pigment adsorption capability, easy regeneration and repeated use, has better decoloring effect and application in decoloring different plant polysaccharides, is influenced by rich functional components and different characteristics of fructus amomi medicinal materials, and has poor decoloring effect by only using resin; and the fructus amomi polysaccharide is affected by the characteristics of the polysaccharide, so that the alcohol solubility of the fructus amomi polysaccharide is poor, and the application range of the fructus amomi polysaccharide is limited.
Therefore, how to separate the fructus amomi polysaccharide from other coloring matters (such as flavonoids, polyphenols and pigments) and reduce the loss of the fructus amomi polysaccharide as much as possible, and improve the alcohol solubility of the polysaccharide so as to widen the application field of the polysaccharide is a problem to be solved.
Disclosure of Invention
The invention aims to provide a preparation method of low-chroma alcohol-soluble fructus amomi polysaccharide extract, aiming at solving the technical problems, thereby obtaining the fructus amomi polysaccharide extract with low chroma, high stability and good alcohol solubility.
The technical scheme provided by the invention is as follows:
A preparation method of low-chroma alcohol-soluble fructus Amomi polysaccharide extract comprises the following steps:
Step one, degreasing: drying fructus Amomi materials in an oven, taking the superfine crushed undersize, dissolving with 1 times 80-95vol% ethanol, soaking for 1-2 hours, performing thermal reflux circulation extraction for 1 time, and collecting filter residues;
step two, extracting: extracting the residue with 45-75vol% ethanol for 1-3 times each for 2-3 hr, separating solid and liquid, collecting filtrate, and concentrating the combined filtrate under reduced pressure;
Step three, acidolysis: adding a certain amount of acid liquor into the concentrated solution, regulating the pH value of the concentrated solution to 2.0-5.0, standing, settling and centrifuging to obtain a centrifugal supernatant;
Step four, anti-solvent precipitation: adding 1-2 times of purified water into the supernatant, standing, settling, centrifuging to obtain a centrifugal supernatant;
step five, resin separation: passing the supernatant through macroporous resin column, collecting the permeate, and concentrating under reduced pressure;
Step six, adjusting pH: adding a certain amount of alkali liquor into the concentrated solution, regulating the pH value of the concentrated solution to 6.0-8.0, standing, settling and centrifuging to obtain a centrifugal supernatant;
step seven, alcohol precipitation: slowly adding the supernatant into absolute ethyl alcohol, wherein the volume ratio of the supernatant to the absolute ethyl alcohol is 1:100-1:300, standing, settling, centrifuging and collecting a precipitate;
Step eight, filter pressing: wrapping the precipitate with filter cloth, placing into a filter press for intermittent filter pressing, and collecting filter cake;
Step nine, freeze drying: freeze-drying the obtained filter cake to obtain a white solid;
Step ten, crushing at low temperature: pulverizing the obtained white solid at-20-0deg.C to obtain low-chroma alcohol-soluble fructus Amomi polysaccharide extract.
Preferably, in the first step, the drying temperature of the medicinal materials is 30-55 ℃ and the drying time is 5-8 hours.
Preferably, in the first step, the pharmacopoeia mesh number used is 30-80 mesh.
Preferably, in the first step, the volume ratio of the medicinal material to the extraction solvent is 1:1-2.
Preferably, in the second step, the volume ratio of the filter residue to the extraction solvent is 1:10-30.
Preferably, in the second step, the extraction temperature of the thermal reflux cycle is 60-95 ℃.
Preferably, in the second step, the extract is concentrated to 1/2 to 1/5 of the original volume.
Preferably, in the third step, the acid solution used includes one or more of citric acid, acetic acid or phosphoric acid.
Preferably, in the third step, the standing sedimentation time is 6 to 24 hours.
Preferably, in the fourth step, the standing time is 12-24 hours.
Preferably, in the fifth step, the resin used is D101, AB-8 or polyamide resin column.
Preferably, in the sixth step, the alkaline reagent is one or more solutions of sodium hydroxide, potassium hydroxide or sodium bicarbonate, and the standing and settling time is 6-12 hours.
Preferably, in the seventh step, the standing time is 12 to 24 hours.
Preferably, in the eighth step, the pressure of the press filtration is 0.3-1.6MPa, and the press filtration time is 10-30 minutes.
Preferably, in the step nine, the filter cake is dried by vacuum freeze-drying or spray freeze-drying.
The invention has the following beneficial effects:
1. The fructus amomi polysaccharide extract prepared by the invention has light color (white powder), high chromaticity stability and good alcohol solubility, and solves the problems of dark color and poor alcohol solubility of the fructus amomi polysaccharide.
2. The equipment for preparing the fructus amomi polysaccharide extract is common, strong acid or toxic organic solvent is not used, the production process is safe and green, and the method is suitable for industrial mass production.
Drawings
FIG. 1 is a graph showing the color difference values and alcohol-soluble extract contents of examples and comparative examples;
fig. 2 is a comparative example and comparative example color chart.
Detailed Description
The present invention will be described in detail with reference to specific examples thereof so as to facilitate the practice of the invention by those skilled in the art with reference to the specification.
Example 1
Taking 1kg of fructus amomi medicinal material after drying and crushing, adding 95% ethanol with the solvent multiple of 1 time, fully mixing, soaking for 1 hour, and heating, refluxing, circulating and degreasing at the temperature of 85 ℃. Adding 60% ethanol with solvent multiple of 15 times into the filter residue, mixing thoroughly, soaking for 1 hr, heating and reflux-extracting for 2 times at 85deg.C for 3 hr/time, mixing 2 times of extractive solutions, and concentrating under reduced pressure. Adding saturated citric acid solution into the concentrated solution, adjusting pH value of the concentrated solution to 3.24, standing at normal temperature for 12 hours, and centrifuging at 4000rpm/min for 15 minutes to obtain supernatant 1. Adding 1.5 times of purified water into the supernatant 1, standing at normal temperature for 12 hours, and centrifuging at 4000rpm/min for 15 minutes to obtain supernatant 2. The supernatant 2 was passed through a D101 macroporous resin column, and the permeate was collected and concentrated under reduced pressure to obtain 560mL of a concentrate. Saturated sodium hydroxide solution was added to the concentrate, the pH of the concentrate was adjusted to 7.2, the concentrate was allowed to stand at normal temperature for 12 hours, and the concentrate was centrifuged at 4000rpm/min for 15 minutes to obtain supernatant 3. 600mL of concentrated solution is slowly added into 84L of absolute ethyl alcohol which is always in a stirring state, after all the concentrated solution is added, the concentrated solution is mechanically stirred for 30 minutes, compressed air is stirred for 10 minutes, the concentrated solution is placed at normal temperature for 24 hours, the concentrated solution is centrifuged for 20 minutes at the centrifugal speed of 4000rpm/min, the precipitate is collected and wrapped by filter cloth, the concentrated solution is put into a filter press for filter pressing, the filter pressing pressure is 1Mpa, the filter pressing time is 20 minutes, and the filter cake is collected. Drying the obtained filter cake in a vacuum freeze dryer for 48 hours, and crushing 116.5g of white solid at the temperature of-20-0 ℃ to obtain 113.2g of low-chroma alcohol-soluble fructus amomi polysaccharide extract.
Example 2
Taking 1kg of fructus amomi medicinal material after drying and crushing, adding 95% ethanol with the solvent multiple of 1 time, fully mixing, soaking for 1 hour, and heating, refluxing, circulating and degreasing at the temperature of 85 ℃. Adding 50% ethanol with solvent multiple of 30 times into the residue, mixing thoroughly, soaking for 1 hr, heating and reflux-extracting for 2 times at 85deg.C for 3 hr/time, mixing 2 times of extractive solutions, and concentrating under reduced pressure. Adding saturated citric acid solution into the concentrated solution, adjusting pH value of the concentrated solution to 2.88, standing at normal temperature for 12 hours, and centrifuging at 4000rpm/min for 15 minutes to obtain supernatant 1. Adding 1.5 times of purified water into the supernatant 1, standing at normal temperature for 12 hours, and centrifuging at 4000rpm/min for 15 minutes to obtain supernatant 2. The supernatant 2 was passed through an AB-8 macroporous resin column, and the permeate was collected and concentrated under reduced pressure to obtain 580mL of a concentrated solution. Saturated sodium hydroxide solution was added to the concentrate, the pH of the concentrate was adjusted to 6.94, the concentrate was allowed to stand at normal temperature for 12 hours, and the concentrate was centrifuged at 4000rpm/min for 15 minutes to give supernatant 3. Slowly adding 615mL of concentrated solution into 100L of absolute ethyl alcohol which is always in a stirring state, mechanically stirring for 30 minutes after all concentrated solutions are added, stirring for 10 minutes by compressed air, standing for 24 hours at normal temperature, centrifuging for 20 minutes at a centrifugal speed of 4000rpm/min, collecting precipitate, wrapping the precipitate with filter cloth, putting into a filter press for filter pressing, wherein the filter pressing pressure is 1.1Mpa, the filter pressing time is 25 minutes, and collecting a filter cake. Drying the obtained filter cake in a vacuum freeze dryer for 48 hours, and crushing 118.2g of white solid at the temperature of-20-0 ℃ to obtain 116.8g of low-chroma alcohol-soluble fructus amomi polysaccharide extract.
Example 3
Taking 1kg of fructus amomi medicinal material after drying and crushing, adding 95% ethanol with the solvent multiple of 1 time, fully mixing, soaking for 1 hour, and heating, refluxing, circulating and degreasing at the temperature of 85 ℃. Adding 55% ethanol with solvent multiple of 20 times into the residue, mixing thoroughly, soaking for 1 hr, heating and reflux-extracting for 2 times at 85deg.C for 3 hr/time, mixing 2 times of extractive solutions, and concentrating under reduced pressure. Adding saturated citric acid solution into the concentrated solution, adjusting pH value of the concentrated solution to 2.55, standing at normal temperature for 12 hours, and centrifuging at 4000rpm/min for 15 minutes to obtain supernatant 1. Adding 1.5 times of purified water into the supernatant 1, standing at normal temperature for 12 hours, and centrifuging at 4000rpm/min for 15 minutes to obtain supernatant 2. The supernatant 2 was passed through a D101 macroporous resin column, and the permeate was collected and concentrated under reduced pressure to obtain 560mL of a concentrate. Saturated sodium hydroxide solution was added to the concentrate, the pH of the concentrate was adjusted to 7.30, the concentrate was allowed to stand at normal temperature for 12 hours, and the concentrate was centrifuged at 4000rpm/min for 15 minutes to obtain supernatant 3. Slowly adding 610mL of concentrated solution into 120L of absolute ethyl alcohol which is always in a stirring state, mechanically stirring for 30 minutes after all concentrated solutions are added, stirring for 10 minutes by compressed air, standing for 24 hours at normal temperature, centrifuging for 20 minutes at a centrifugal speed of 4000rpm/min, collecting precipitate, wrapping the precipitate by using filter cloth, putting into a filter press for filter pressing, wherein the filter pressing pressure is 0.9Mpa, the filter pressing time is 20 minutes, and collecting a filter cake. Drying the obtained filter cake in a vacuum freeze dryer for 48 hours, and crushing 120.4g of white solid at the temperature of-20-0 ℃ to obtain 119.2g of low-chroma alcohol-soluble fructus amomi polysaccharide extract.
Comparative example 1
The difference compared to example 3 is that the raw material is not subjected to degreasing treatment.
Comparative example 2
In comparison with example 3, the difference is that the extract is not acidolyzed.
Comparative example 3
The difference compared to example 3 is that the ethanol precipitation is carried out using 95% ethanol.
Comparative example 4
The difference compared to example 3 is that no filter press technique is used.
Comparative example 5
The difference compared to example 3 is that the extraction solvent is purified water.
Comparative example 6
The preparation is carried out according to the technology published by CN 201610350733.7: taking 1kg of fructus amomi medicinal material, crushing the fructus amomi medicinal material by using a crusher, adding the crushed fructus amomi medicinal material into a volatile oil extractor, adding 10L of purified water, soaking for 0.5 hour, heating and extracting for 5.0 hours, collecting an extracted crude liquid, centrifuging for 15 minutes at a centrifugal speed of 4000rpm/min, collecting a centrifugal supernatant, concentrating under reduced pressure, adding 1700mL of 95% ethanol into the concentrated liquid, wherein the mass fraction of the ethanol in the concentrated liquid reaches 60%, standing for 24 hours, centrifuging for 20 minutes at a centrifugal speed of 4000rpm/min, collecting a precipitate, drying in a plate-type vacuum dryer, crushing, and sieving with a 80-mesh sieve to obtain 50.3g of brown yellow fructus amomi polysaccharide extract.
Test example 1
The light source is set as D 65, a view angle of 10 degrees is selected as a view field, the aperture is measured to be 4mm, the light source LED emits blue laser, and a black-and-white plate is used for calibrating the color difference meter. Samples of experimental example 3, comparative example 1, comparative example 2, comparative example 3, comparative example 4, comparative example 5, and comparative example 6 (sieved with a No. 4 sieve) were taken, put into a color meter, and evenly spread on the bottom for sample measurement.
Test example 2: about 2-4g of the sample is taken, precisely weighed and placed in a conical flask with the volume of 100-250mL, 50-100mL of 60% ethanol is precisely added, the flask is sealed, the weight is weighed, the flask is kept stand for 1 hour, then the flask is connected with a reflux condenser tube, heated to be boiling, and micro boiling is kept for 1 hour. After cooling, the conical flask is taken down, the sealing is carried out, the weight is weighed again, the weight loss is complemented by 60% ethanol, the shaking is carried out, the filtering is carried out by a drying filter, 25mL of filtrate is precisely measured, the filtrate is placed in an evaporation dish which is dried to constant weight, the evaporation dish is dried by water bath, the water bath is dried for 3 hours, the water bath is cooled for 30 minutes, the weight is rapidly and precisely weighed, and the content (%) of the alcohol-soluble extract in the sample is calculated by the dried product.
TABLE 1 color difference values of the samples and results of data on the content of alcohol-soluble extract
As can be seen from the combination of Table 1 and FIGS. 1-2, the sample chromaticity L * of the fructus Amomi polysaccharide extract prepared in examples 1, 2 and 3 is higher and has a smaller difference from the content of the alcohol-soluble extract, which indicates that the preparation method of the low chromaticity alcohol-soluble fructus Amomi polysaccharide extract is stable and reliable. Comparative example 6 was prepared according to the disclosed polysaccharide extract process from amomum villosum, with both the color intensity L * and the alcohol-soluble extract content significantly lower than in experimental example 3; after one process is reduced or modified in comparative examples 1, 2,3, 4 and 5, the L * value and the alcohol-soluble extract content of the obtained fructus amomi polysaccharide extract are obviously reduced, wherein the comparative example 5 only changes the extraction solvent, other processes are consistent with the experimental example 3, and the fructus amomi polysaccharide extract with low chromaticity can still be obtained, but the alcohol solubility is lower than that of the experimental example 3, so that the preparation process of the low-purity fructus amomi polysaccharide extract provided by the invention has relativity, uniqueness and uniqueness.
The above examples are merely illustrative of preferred embodiments of the present invention and do not include all embodiments of the invention. Various modifications and alterations may be made by those skilled in the art without departing from the spirit and scope of the invention, which is to be considered as falling within the scope of the appended claims.
Claims (10)
1. A preparation method of low-chroma alcohol-soluble fructus amomi polysaccharide extract is characterized by comprising the following steps:
Step one, degreasing: drying fructus Amomi materials in an oven, taking the superfine crushed undersize, dissolving with 1 times 80-95vol% ethanol, soaking for 1-2 hours, performing thermal reflux circulation extraction for 1 time, and collecting filter residues;
step two, extracting: extracting the residue with 45-75vol% ethanol for 1-3 times each for 2-3 hr, separating solid and liquid, collecting filtrate, and concentrating the combined filtrate under reduced pressure;
Step three, acidolysis: adding a certain amount of acid liquor into the concentrated solution, regulating the pH value of the concentrated solution to 2.0-5.0, standing, settling and centrifuging to obtain a centrifugal supernatant;
Step four, anti-solvent precipitation: adding 1-2 times of purified water into the supernatant, standing, settling, centrifuging to obtain a centrifugal supernatant;
step five, resin separation: passing the supernatant through macroporous resin column, collecting the permeate, and concentrating under reduced pressure;
Step six, adjusting pH: adding a certain amount of alkali liquor into the concentrated solution, regulating the pH value of the concentrated solution to 6.0-8.0, standing, settling and centrifuging to obtain a centrifugal supernatant;
step seven, alcohol precipitation: slowly adding the supernatant into absolute ethyl alcohol, wherein the volume ratio of the supernatant to the absolute ethyl alcohol is 1:100-1:300, standing, settling, centrifuging and collecting a precipitate;
Step eight, filter pressing: wrapping the precipitate with filter cloth, placing into a filter press for intermittent filter pressing, and collecting filter cake;
Step nine, freeze drying: freeze-drying the obtained filter cake to obtain a white solid;
Step ten, crushing at low temperature: pulverizing the obtained white solid at-20-0deg.C to obtain low-chroma alcohol-soluble fructus Amomi polysaccharide extract.
2. The method according to claim 1, wherein in the first step, the drying temperature of the medicinal material is 30-55 ℃ and the drying time is 5-8 hours; the mesh number of the pharmacopoeia is 30-80 mesh; the volume ratio of the medicinal materials to the extracting solvent is 1:1-2.
3. The method according to claim 1, wherein in the second step, the volume ratio of the filter residue to the extraction solvent is 1:10-30 parts of a base; the extraction temperature of the thermal reflux circulation is 60-95 ℃; concentrating the extractive solution to 1/2-1/5 of the original volume.
4. The method according to claim 1, wherein in the third step, the acid solution used comprises one or more of citric acid, acetic acid and phosphoric acid; the standing sedimentation time is 6-24 hours.
5. The method according to claim 1, wherein in the fourth step, the standing time is 12 to 24 hours.
6. The method according to claim 1, wherein in the fifth step, the resin used is D101, AB-8 or a polyamide resin column.
7. The method according to claim 1, wherein in the sixth step, the alkaline agent is one or more of sodium hydroxide, potassium hydroxide and sodium bicarbonate, and the settling time is 6-12 hours.
8. The method according to claim 1, wherein in the seventh step, the standing time is 12 to 24 hours.
9. The method according to claim 1, wherein in the eighth step, the pressure filtration is 0.3 to 1.6MPa and the time of the pressure filtration is 10 to 30 minutes.
10. The method of claim 1, wherein in step nine, the filter cake is dried by vacuum freeze-drying or spray freeze-drying.
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