CN113527527A - Method for extracting algal polysaccharide through continuous phase change - Google Patents
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Abstract
The invention belongs to the technical field of natural product extraction, and particularly relates to a method for extracting algal polysaccharide through continuous phase change, which comprises the following steps: s1, drying the laver and crushing to obtain a dry laver raw material; s2, putting dry laver into an extraction kettle of a continuous phase change extraction device, compressing an extractant into liquid by a high-pressure pump under the condition that the pressure and the temperature of the extractant are always lower than the critical pressure and the critical temperature of the extractant, extracting algal polysaccharide by flowing through the extraction kettle at a certain flow rate, then entering an analytical kettle, changing the phase of the extractant into gas by heating and reducing pressure, then immediately compressing the gas to form liquid, flowing through the extraction kettle, extracting the material again, and circulating for multiple times, wherein the extractant is water. The invention has high extraction rate, and the extractant can be recycled. Compared with the conventional hot water extraction method, the yield of the algal polysaccharide is improved by 5-10%, and the extraction time is shortened by 40-60%.
Description
Technical Field
The invention relates to the technical field of natural product extraction, in particular to a method for extracting algal polysaccharide through continuous phase change.
Background
"ocean economy is an essential component of the global life support system and is also a valuable asset that helps to realize sustainable development. At present, the marine drugs approved as 'quasi' characters in China include alginic acid diester sodium, glucitol, polyene kang, mannitol nicotinate, duokang, hydrate, cadikon, lovastatin, glucose-lowering Ningsan and the like.
With the improvement of the quality of life of people, health food is more and more generally entering the families of common people. The marine organism contains rich high-quality protein, unsaturated fatty acid, vitamins, minerals, dietary fiber and various unique bioactive substances, and has effects of nourishing brain, improving intelligence, preventing tumor, preventing cardiovascular and cerebrovascular diseases, inhibiting bacteria and virus, regulating blood pressure, regulating blood sugar, regulating immunity, and resisting aging. At present, marine algae, fish, mollusks, echinoderm, coelenterate, crustacean resources and the like are utilized in China and are combined with traditional Chinese medicine resources to develop various series of marine health-care foods. Therefore, the method has great market potential for the efficient extraction of marine algae.
Disclosure of Invention
The invention aims to improve the extraction rate of algal polysaccharide, simplify the complicated subsequent refining process and provide a method for continuous phase change extraction of algal polysaccharide, which has high extraction rate, high purity of polysaccharide, safety, environmental protection and lower cost and is suitable for large-scale industrial production.
In order to achieve the purpose, the invention provides the following technical scheme:
a method for extracting algal polysaccharides through continuous phase change comprises the following steps:
s1, drying the laver and crushing to obtain a dry laver raw material;
s2, dry laver is put into an extraction kettle of a continuous phase change extraction device, under the condition that the pressure and the temperature of the extraction agent are always lower than the critical pressure and the critical temperature of the extraction agent, a high-pressure pump compresses the extraction agent into liquid, the liquid flows through the extraction kettle at a certain flow rate to extract algal polysaccharide, then the liquid enters an analytic kettle, the extraction agent is heated and decompressed to be changed into gas, the gas is then compressed immediately, the gas is changed into liquid, the liquid flows through the extraction kettle to extract the material again, the cycle is repeated, the extraction agent refers to water, and the extraction condition is as follows: the extraction temperature is 60-100 ℃, the extraction pressure is 0.2-0.5 Mpa, the continuous extraction is carried out for 180-300 min, the flow rate is 20-100L/h, the resolution temperature is 60-100 ℃, and the resolution pressure is-0.08 Mpa.
In a preferred embodiment of the present invention, the extraction temperature is 60-100 ℃, the extraction time is 180-300 min, the extraction flow rate is 20L/h-100L/h, and the extraction flow rate is preferably 40L/h-80L/h.
In the preferred embodiment of the invention, the extraction temperature is 80 ℃, the extraction time is 240min, the extraction flow rate is 60L/h, and the extraction pressure is 0.20 MPa.
In the preferred embodiment of the invention, the extraction temperature is 90 ℃, the extraction time is 180min, the extraction flow rate is 80L/h, and the extraction pressure is 0.3 MPa.
In the preferred embodiment of the invention, the extraction temperature is 100 ℃, the extraction time is 300min, the extraction flow rate is 100L/h, and the extraction pressure is 0.35 MPa.
In a preferred embodiment of the invention, the drying temperature is 50-60 ℃, and the moisture content is controlled to be 8-15%.
In a preferred embodiment of the present invention, the ratio of the liquid to the material in step S2 is 1: 10-150.
In a preferred embodiment of the invention, the seaweed is dried at a temperature of 55 ℃ and the moisture content is controlled to 10%.
In the preferred embodiment of the invention, the desorption temperature is 80 ℃ and the desorption pressure is-0.08 MPa.
In a preferred embodiment of the present invention, the pH of the extractant is tertiary water with 5.0 to 7.5.
The continuous phase change technology adopted by the invention is a process that an extracting agent flows through an extraction kettle under certain pressure and temperature conditions to extract materials, then the materials are subjected to phase change into gas through a resolving device, the extracted materials fall into the resolving kettle, the resolved gas is condensed into liquid and flows through the extraction kettle again to extract the materials repeatedly, and the materials can be continuously extracted for many times in a dynamic and efficient manner. Compared with the traditional hot water extraction method, the method has the characteristics of high extraction rate of effective components, almost no consumption and pollution of solvent in the extraction process, quick action effect, low energy consumption, large treatment capacity, low production cost and the like.
Compared with the traditional solvent, supercritical extraction technology and subcritical extraction technology, the continuous phase-change extraction technology has the advantages of high efficiency of supercritical extraction and subcritical extraction, no solvent residue in the product, high aroma component retention rate, low extraction pressure and desorption pressure compared with the supercritical extraction technology, and has the characteristics of large volume, large batch processing capacity, low production cost and the like of the conventional solvent extraction. In addition, the continuous phase-change extraction also has the advantages of short extraction time, realization of an instant continuous extraction process, less solvent requirement, solvent recovery and the like. In the whole extraction process, the phase change process of the extractant from liquid to gas to liquid is instant and continuous. The extraction agent is subjected to continuous phase change and is recycled, the algal polysaccharide is stored in an analysis kettle, and is discharged and collected after extraction.
Compared with the prior art, the invention has the following advantages:
1. the invention adopts the continuous phase-change extraction and separation technology, not only effectively reduces the production cost, shortens the extraction and separation time, and reduces the solvent consumption and energy consumption in the process, but also has simple process flow, strong operability, high extraction efficiency, environmental protection, no pollution, good completeness and repeatability, and can realize large-scale industrial continuous production;
2. the whole extraction process is carried out under the conditions of closed oxygen insulation, high temperature and high pressure, so the method is particularly suitable for the industrial continuous production of the algal polysaccharide;
3. the invention has high extraction rate, and the extractant can be recycled. Compared with the conventional method, the extraction rate of the algal polysaccharide is improved by 5-10%, the extraction rate can reach more than 15%, and the extraction time can be shortened by about 40-60%.
Drawings
FIG. 1 is a graph showing the effect of extraction time on polysaccharide extraction yield.
FIG. 2 is a graph showing the effect of extraction temperature on polysaccharide extraction yield.
Detailed Description
The technical solutions of the present invention will be described clearly and completely with reference to the following embodiments of the present invention, and it should be understood that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention. The examples, in which specific conditions are not specified, were conducted under conventional conditions or conditions recommended by the manufacturer. The reagents or instruments used are not indicated by the manufacturer, and are all conventional products available commercially.
Solid content and polysaccharide content detection and yield comparison
The polysaccharide detection method comprises the following steps: phenol-sulfuric acid process
(1) Principle of
The sulfuric acid solution with a certain concentration can hydrolyze polysaccharide into monosaccharide or oligosaccharide, the monosaccharide or oligosaccharide is immediately dehydrated to generate a furfural derivative, the derivative is condensed into an orange-yellow stable compound when meeting phenol, the compound has maximum absorption at 490nm, the absorption value and the polysaccharide content are in a linear relation, and the polysaccharide content can be calculated through the absorption value.
(2) Pretreatment of raw materials
Taking 5.00g of pretreated seaweed raw material, and mixing the raw material according to the proportion of 1: 150mL of distilled water was added at a feed-to-liquid ratio of 30(m: V). Performing ultrasonic treatment for 20min at 40Hz, and extracting for 1.5h under magnetic stirring in 80 deg.C constant temperature water bath; centrifuging at 4000 r/min for 10 min. Extracting twice, squeezing and filtering with 120 mesh nylon gauze, and concentrating the filtrate in a 50 deg.C drying oven.
(3) Preparation of Standard Curve
Taking a proper amount of an anhydrous D-galactose reference substance, precisely weighing, and adding water to prepare a solution containing 0.6mg of anhydrous D-galactose per 1 mL. Precisely measuring the reference substance solutions 1.0mL, 1.5mL, 2.0mL, 2.5mL, 3.0mL and 4.0mL, respectively placing in 50mL measuring bottles, adding water to the scale, and shaking. Precisely measuring 2mL of each solution, placing the solution in a test tube with a plug, respectively adding 1mL of 6% phenol solution, uniformly mixing, quickly adding 5.0mL of sulfuric acid, shaking uniformly, boiling in a boiling water bath for 10min, taking out, placing in an ice water bath, cooling, taking out, taking corresponding reagents as blanks, measuring absorbance at 490nm wavelength by an ultraviolet-visible spectrophotometry (general rule 0401), taking the absorbance as an ordinate, and taking the concentration as an abscissa, and drawing a standard curve.
(4) Sample assay
Precisely measuring 2g of the extractive solution or concentrated solution, adding 10mL of ethanol, stirring, standing in a refrigerator at 4 deg.C for more than 2h (overnight is recommended), centrifuging (setting 4000 r 10min for centrifugation), washing precipitate with 5mL of 80% ethanol solution, centrifuging, discarding supernatant, and performing 2 times. Dissolving in water, placing in a 50mL volumetric flask, diluting to a scale (if the detected light absorption value is too high, then diluting on the basis, if the detected light absorption value is too low, then increasing the pretreatment sampling amount of pretreatment), shaking uniformly, placing 2mL precisely, measuring the absorbance by the method from the point of adding 1mL of 6% phenol solution according to the preparation method of the standard curve, reading the concentration (mg/mL) of anhydrous D-galactose in the reference solution from the standard curve, and calculating to obtain the D-galactose.
(5) Calculation of results
The content of total polysaccharide in the extract (mg/g) ═ CSample (A)×V1×N)/M1
In the formula: cSample (A)- [ polysaccharide concentration in the polysaccharide concentration in the sample;
V1the volume of the crude polysaccharide solution of the test solution is mL;
n-dilution multiple;
M1-;
two measurements were performed in parallel and the average was reported. The relative error is less than or equal to 5 percent.
Detection and calculation:
example 1A method for continuous phase transition extraction of algal polysaccharides
1. A method for extracting algal polysaccharides through continuous phase change comprises the following steps:
(1) drying thallus Porphyrae at 55 deg.C, controlling water content at 10%, and pulverizing to obtain dried thallus Porphyrae material;
(2) taking 10kg of the treated dry laver, loading the dried laver into an extraction kettle of a continuous phase change extraction device, compressing an extractant into liquid by a high-pressure pump under the condition that the pressure and the temperature of the extractant are always lower than the critical pressure and the critical temperature of the extractant, extracting the seaweed oil by flowing through the extraction kettle at a certain flow rate, entering an analytic kettle, changing the phase of the extractant into gas by heating and decompressing, then immediately compressing the gas to form liquid, flowing through the extraction kettle, extracting the material again, and repeating the steps for many times, wherein the extractant is water, and the extraction conditions are as follows: extracting at 80 deg.C under 0.2Mpa for 240min at 100L/h flow rate, and at 80 deg.C under 0.1 Mpa; the feed-liquid ratio of the raw material to the extracting agent is 1:10 (g/mL).
(3) After extraction, the extract solution flows through an analysis kettle, the analysis temperature is set at 80 ℃, the analysis pressure is-0.08 MPa, the seaweed polysaccharide extract is discharged from the analysis kettle, pure water is recovered and collected, and the seaweed solid and polysaccharide content are detected.
Comparative example 1 extraction method for extracting algal polysaccharide by hot water extraction
(1) Drying thallus Porphyrae at 55 deg.C, controlling water content at 10%, and pulverizing to obtain dried thallus Porphyrae material;
(2) adding 1kg of the treated dry laver into a conventional extraction tank, adding 40L of tertiary water, wherein the material-liquid ratio of the raw material to the extracting agent is 1: and 40, heating and extracting, wherein the designed extraction temperature is 80 ℃, the extraction time is 240min, and the solid content and the polysaccharide content of the seaweed are detected after extraction.
TABLE 1 comparison of solid yield and polysaccharide yield obtained by different extraction processes
As can be seen from Table 1, the results show that, compared with the hot water extraction process, the solid content and polysaccharide yield of the continuous phase change extraction process of Ganoderma lucidum is respectively improved by 9% and 5.08%, and the solid content and polysaccharide yield of the continuous phase change extraction process is significantly higher than that of the conventional hot water extraction process.
EXAMPLE 2 study of continuous phase transition extraction method of algal polysaccharides
The invention continuously analyzes, determines and adjusts the process conditions according to the characteristics of the seaweed raw material. Operating with reference to the following steps:
(1) drying thallus Porphyrae at 55 deg.C, controlling water content at 10%, and pulverizing to obtain dried thallus Porphyrae material;
(2) adding 2000g of dried laver raw material into a 20L extraction kettle, determining the extraction pressure to be 0.20MPa, the extraction flow rate to be 60L/h, setting the extraction temperature and the extraction time, and injecting pure water into the extraction kettle.
(3) After extraction, the extract solution flows through an analysis kettle, the analysis temperature is set at 80 ℃, the analysis pressure is-0.08 MPa, the seaweed polysaccharide extract is discharged from the analysis kettle, pure water is recovered and collected, and the seaweed solid and polysaccharide content are detected.
The attached figures 1-2 provide the results of the influence of extraction time, extraction temperature and extraction rate on algal polysaccharide. Table 2 shows the effect of extraction temperature on algal polysaccharide extraction rate, and Table 3 shows the effect of extraction time on algal polysaccharide extraction rate.
The influence of the extraction time on the extraction rate of algal polysaccharides is shown in figure 1, and the extraction time is 60-300 min. When the extraction time is 60-300 min, the extraction rate of algal polysaccharide is obviously increased along with the increase of the extraction time, the extraction rate of polysaccharide reaches the maximum value when the extraction time is 120min, and the ratio of raw materials to extracting agent is 14.29%, wherein the ratio of raw materials to extracting agent is 1: 60. however, the research of the invention finds that the longer the extraction time is, the better the extraction time is, the polysaccharide extraction rate is not increased obviously and the seaweed polysaccharide is decomposed along with the extension of the extraction time, and the process cost is obviously increased.
The influence of the extraction temperature on the extraction rate of algal polysaccharides is shown in figure 2, and the extraction time is 60-100 ℃. The influence of the extraction temperature on the extraction rate of the algal polysaccharide is that when the temperature range is between 60 ℃ and 100 ℃, the extraction rate of the algal polysaccharide is obviously increased along with the increase of the extraction temperature, and under the condition that the same extraction time is 180min, the extraction rate of the polysaccharide reaches the maximum value of 15.61% when the extraction temperature is 80 ℃. However, the present inventors have found that it is not preferable to increase the extraction temperature, and that excessive temperature may destroy the decomposition of algal polysaccharides, and at the same time, the high temperature may increase energy consumption and increase the cost.
TABLE 2 Effect of extraction temperature on algal polysaccharide extraction yield
TABLE 3 Effect of extraction time on algal polysaccharide extraction yield
Example 3A method for continuous phase transition extraction of algal polysaccharides
(1) Drying thallus Porphyrae at 55 deg.C, controlling water content at 13%, and pulverizing to obtain dried thallus Porphyrae material;
(2) adding 2000g of dry laver raw material into a 20L extraction kettle, injecting three-level pure water with the pH value of 7.0 into the extraction kettle at the extraction temperature of 80 ℃, the pressure of 0.10MPa and the extraction flow rate of 40L/h, and continuously extracting for 240min, wherein the material-liquid ratio of the raw material to the extracting agent is 1: 80;
(3) after extraction, the extract solution flows through an analysis kettle, the analysis temperature is set at 80 ℃, the analysis pressure is-0.08 MPa, the algal polysaccharide extract is discharged from the analysis kettle, pure water is recovered and collected, and the yield of the algal polysaccharide is detected to be 15.16%.
Example 4A method for continuous phase transition extraction of algal polysaccharides
(1) Drying thallus Porphyrae at 55 deg.C, controlling water content at 13%, and pulverizing to obtain dried thallus Porphyrae material;
(2) adding 2000g of dry laver raw material into a 20L extraction kettle, injecting three-level pure water with the pH value of 7.2 into the extraction kettle at the extraction temperature of 100 ℃, the pressure of 0.2MPa and the extraction flow rate of 60L/h, and continuously extracting for 180min, wherein the material-liquid ratio of the raw material to the extracting agent is 1: 90, respectively;
(3) after extraction, the extract solution flows through an analysis kettle, the analysis temperature is set at 80 ℃, the analysis pressure is-0.08 MPa, the seaweed polysaccharide extract is discharged from the analysis kettle after extraction is finished, pure water is recovered, and the polysaccharide yield is 14.01%.
Example 5A method for continuous phase transition extraction of algal polysaccharides
(1) Drying thallus Porphyrae at 50 deg.C, controlling water content at 8%, and pulverizing to obtain dried thallus Porphyrae material;
(2) adding 2000g of dry laver raw material into a 20L extraction kettle, injecting three-level pure water with the pH of 7.2 into the extraction kettle at the extraction temperature of 100 ℃, the pressure of 0.2MPa and the extraction flow rate of 60L/h, and continuously extracting for 300min, wherein the material-liquid ratio of the raw material to the extracting agent is 1: 150;
(3) after extraction, the extract solution flows through an analysis kettle, the analysis temperature is set at 80 ℃, the analysis pressure is-0.08 MPa, the seaweed polysaccharide extract is discharged from the analysis kettle after extraction is finished, pure water is recovered, and the polysaccharide yield is 12.96%.
Example 6A method for continuous phase transition extraction of algal polysaccharides
(1) Drying thallus Porphyrae at 50 deg.C, controlling water content at 10%, and pulverizing to obtain dried thallus Porphyrae material;
(2) adding 2000g of dry laver raw material into a 20L extraction kettle, injecting three-level pure water with the pH of 7.2 into the extraction kettle at the extraction temperature of 80 ℃, the pressure of 0.2MPa and the extraction flow rate of 60L/h, and continuously extracting for 180min, wherein the material-liquid ratio of the raw material to the extracting agent is 1: 90, respectively;
(3) after extraction, the extract solution flows through an analysis kettle, the analysis temperature is set at 80 ℃, the analysis pressure is-0.08 MPa, the seaweed polysaccharide extract is discharged from the analysis kettle after extraction is finished, pure water is recovered, and the polysaccharide yield is 17.1%.
The embodiments of the present invention have been described in detail, but the present invention is not limited to the described embodiments. It will be apparent to those skilled in the art that various changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, and the scope of protection is still within the scope of the invention.
Claims (7)
1. A method for extracting algal polysaccharide through continuous phase change is characterized by comprising the following steps:
s1, drying the laver and crushing to obtain a dry laver raw material;
s2, dry laver is put into an extraction kettle of a continuous phase change extraction device, under the condition that the pressure and the temperature of the extraction agent are always lower than the critical pressure and the critical temperature of the extraction agent, a high-pressure pump compresses the extraction agent into liquid, the liquid flows through the extraction kettle at a certain flow rate to extract algal polysaccharide, then the liquid enters an analytic kettle, the extraction agent is heated and decompressed to be changed into gas, the gas is then compressed immediately, the gas is changed into liquid, the liquid flows through the extraction kettle to extract the material again, the cycle is repeated, the extraction agent refers to water, and the extraction condition is as follows: the extraction temperature is 60-100 ℃, the extraction pressure is 0.2-0.5 Mpa, the continuous extraction is carried out for 180-300 min, the flow rate is 20-100L/h, the resolution temperature is 60-100 ℃, and the resolution pressure is-0.08 Mpa.
2. The method for continuous phase transition extraction of algal polysaccharides according to claim 1, wherein the laver is dried at a temperature of 40 to 60 ℃ and the moisture content is controlled to 8 to 15% and crushed in step S1.
3. The method for continuous phase change extraction of algal polysaccharides according to claim 1, wherein the extraction temperature is 80 ℃, the extraction time is 240min, the extraction flow rate is 60L/h, and the extraction pressure is 0.20 MPa.
4. The method for continuous phase change extraction of algal polysaccharides according to claim 1, wherein the extraction temperature is 90 ℃, the extraction time is 180min, the extraction flow rate is 80L/h, and the extraction pressure is 0.30 MPa.
5. The method for continuous phase change extraction of algal polysaccharides according to claim 1, wherein the extraction temperature is 100 ℃, the extraction time is 300min, the extraction flow rate is 100L/h, and the extraction pressure is 0.35 MPa.
6. The method for continuous phase-change extraction of algal polysaccharides according to claim 1, wherein the desorption temperature is 80 ℃ and the desorption pressure is-0.08 MPa.
7. The method for continuous phase-change extraction of algal polysaccharides according to claim 1, wherein the ratio of the material to the liquid in step S2 is 1: 10-150.
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Application publication date: 20211022 |