CN115197337A - High-pressure blasting-based extraction process of green alga polysaccharide - Google Patents
High-pressure blasting-based extraction process of green alga polysaccharide Download PDFInfo
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- CN115197337A CN115197337A CN202210785899.7A CN202210785899A CN115197337A CN 115197337 A CN115197337 A CN 115197337A CN 202210785899 A CN202210785899 A CN 202210785899A CN 115197337 A CN115197337 A CN 115197337A
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- 150000004676 glycans Chemical class 0.000 title claims abstract description 43
- 229920001282 polysaccharide Polymers 0.000 title claims abstract description 43
- 239000005017 polysaccharide Substances 0.000 title claims abstract description 43
- 238000000605 extraction Methods 0.000 title claims abstract description 36
- 238000005422 blasting Methods 0.000 title claims abstract description 35
- 239000007790 solid phase Substances 0.000 claims abstract description 17
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 17
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims abstract description 16
- 239000000725 suspension Substances 0.000 claims abstract description 16
- 241000195649 Chlorella <Chlorellales> Species 0.000 claims abstract description 13
- 238000006243 chemical reaction Methods 0.000 claims abstract description 13
- 239000007788 liquid Substances 0.000 claims abstract description 13
- 239000000843 powder Substances 0.000 claims abstract description 13
- 241000195628 Chlorophyta Species 0.000 claims abstract description 12
- 238000001035 drying Methods 0.000 claims abstract description 12
- 239000012153 distilled water Substances 0.000 claims abstract description 11
- 238000007873 sieving Methods 0.000 claims abstract description 11
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 8
- 239000007791 liquid phase Substances 0.000 claims abstract description 8
- 239000003208 petroleum Substances 0.000 claims abstract description 8
- 238000004140 cleaning Methods 0.000 claims abstract description 7
- 239000012535 impurity Substances 0.000 claims abstract description 7
- 238000005406 washing Methods 0.000 claims abstract description 7
- 238000000926 separation method Methods 0.000 claims abstract description 6
- 239000007787 solid Substances 0.000 claims description 12
- 238000000034 method Methods 0.000 claims description 11
- 239000000706 filtrate Substances 0.000 claims description 7
- 239000002244 precipitate Substances 0.000 claims description 7
- 238000010992 reflux Methods 0.000 claims description 7
- 238000010298 pulverizing process Methods 0.000 claims description 6
- 238000003828 vacuum filtration Methods 0.000 claims description 6
- 238000001816 cooling Methods 0.000 claims description 5
- 238000005238 degreasing Methods 0.000 claims description 4
- 238000001914 filtration Methods 0.000 claims description 4
- 241000195493 Cryptophyta Species 0.000 claims description 2
- 235000011837 pasties Nutrition 0.000 claims description 2
- 238000004880 explosion Methods 0.000 claims 1
- 230000001376 precipitating effect Effects 0.000 abstract description 4
- 229920002522 Wood fibre Polymers 0.000 abstract 1
- 239000002657 fibrous material Substances 0.000 abstract 1
- 239000000126 substance Substances 0.000 abstract 1
- 239000002025 wood fiber Substances 0.000 abstract 1
- 239000000835 fiber Substances 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 239000002002 slurry Substances 0.000 description 3
- 238000005119 centrifugation Methods 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 241000206761 Bacillariophyta Species 0.000 description 1
- 241001474374 Blennius Species 0.000 description 1
- 229920002488 Hemicellulose Polymers 0.000 description 1
- AEMOLEFTQBMNLQ-BKBMJHBISA-N alpha-D-galacturonic acid Chemical group O[C@H]1O[C@H](C(O)=O)[C@H](O)[C@H](O)[C@H]1O AEMOLEFTQBMNLQ-BKBMJHBISA-N 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000009172 bursting Effects 0.000 description 1
- 239000002537 cosmetic Substances 0.000 description 1
- 230000006378 damage Effects 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 235000013305 food Nutrition 0.000 description 1
- 238000007654 immersion Methods 0.000 description 1
- 229920005610 lignin Polymers 0.000 description 1
- 235000016709 nutrition Nutrition 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 238000012916 structural analysis Methods 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- 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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- Health & Medical Sciences (AREA)
- Engineering & Computer Science (AREA)
- Molecular Biology (AREA)
- General Health & Medical Sciences (AREA)
- Sustainable Development (AREA)
- Biochemistry (AREA)
- Materials Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Polysaccharides And Polysaccharide Derivatives (AREA)
Abstract
The invention relates to a high-pressure blasting-based extraction process of green alga polysaccharide, belonging to the technical field of extraction of green alga polysaccharide. Firstly, removing impurities from green algae, cleaning, drying, crushing, and sieving with a 100-mesh sieve; then putting the powder into K 2 CO 3 Preparing the solution into a suspension and carrying out reaction; then carrying out high-pressure blasting reaction on the suspension; then carrying out solid-liquid separation on the reacted substances, and respectively collecting solid-phase samples and liquid-phase samples; washing the solid phase sample with distilled water, and then drying and crushing; defatting with petroleum ether, reflux-extracting with hot water, concentrating the extractive solution under reduced pressure, precipitating with anhydrous ethanol, and centrifuging to obtain Chlorella polysaccharide. The ultramicro structure of the wood fiber is destroyed by high-pressure blasting, the characteristics of the fiber material are changed, and the effective large-heat extraction action area is realized, so that the efficiency of the green alga polysaccharide is obviously improved.
Description
Technical Field
The invention belongs to the technical field of extraction of green alga polysaccharides, and particularly relates to a high-pressure blasting-based extraction process of green alga polysaccharides.
Background
The green algae, as a macro algae widely distributed, has significant differences in nutritional and medicinal values from terrestrial plants due to their existence in special environments such as high salt, high pressure and low light. Polysaccharides are important components of green algae and are widely applied in the industries of food, medicine, cosmetics, cultivation and the like.
The traditional polysaccharide extraction methods include hot water reflux method and immersion extraction method. However, the structure of the green alga polysaccharide is complex, the structural analysis is complicated, and especially the difficulty of the analysis of the high-grade structure is high, so that the extraction rate of the green alga polysaccharide by the traditional extraction process is low.
Disclosure of Invention
In order to solve the problems, the invention provides a high-pressure blasting-based green alga polysaccharide extraction process. Solves the problem of low extraction rate of the green alga polysaccharide extracted by the traditional method.
In order to achieve the purpose, the invention is implemented according to the following technical scheme:
a process for extracting Chlorella polysaccharide based on high pressure blasting comprises the following steps,
s1: removing impurities from green algae, cleaning, drying, pulverizing, and sieving with 100 mesh sieve;
s2: taking the sieved powder, adding 0.2% of K 2 CO 3 Preparing solution into suspension of 3% W/V, thermally reacting at 120 deg.C for 20min, and naturally cooling to room temperature to obtain dark green suspension;
s3: and (3) carrying out high-pressure blasting reaction on the cooled suspension: pressurizing to 80MPa, and rapidly releasing pressure;
s4: carrying out vacuum filtration on the dark green viscous pasty liquid subjected to high-pressure blasting to realize liquid-solid separation, and respectively collecting a solid-phase sample and a liquid-phase sample;
s5: washing the solid phase sample for multiple times by using distilled water until the pH value of the washed distilled water is 6-7, then placing the solid phase sample in an environment of 80 ℃ for drying until the quality is unchanged, and then crushing the solid phase sample and sieving the crushed solid phase sample by using a 100-mesh sieve;
s6, degreasing the sieved solid powder by using petroleum ether, wherein the solid-liquid ratio is 1g: 20-50 mL, and then carrying out heat extraction at 50-80 ℃ for 120min;
s7, carrying out vacuum filtration on an extracting solution obtained by refluxing during hot extraction, carrying out vacuum concentration on a filtrate, adding absolute ethyl alcohol to precipitate polysaccharide, and centrifuging to obtain a precipitate, namely green alga polysaccharide;
s8: concentrating the liquid phase sample under reduced pressure, adding anhydrous ethanol to precipitate polysaccharide, and centrifuging to obtain precipitate as Chlorella polysaccharide.
Preferably, in step S1, the selected green algae species are blue algae or diatoms.
Preferably, in step S3, the suspension is put into a high-pressure homogenizer for high-pressure blasting reaction, the flow rate is 10L/h, the blasting pressure is 80MPa, and the pressure relief time is not more than 5S.
Preferably, in step S6, the solid-to-liquid ratio of the solid powder to the petroleum ether is 1g:40mL; the heat extraction temperature is 60 deg.C, and the time is 90min.
Preferably, in step S7, the filtrate is concentrated under reduced pressure to 1/20 of the original extract, the centrifugation speed is 6000r/min, and the centrifugation time is 10min.
The invention has the beneficial effects that:
1. the superfine structure of the fiber can be obviously destroyed through high-pressure blasting, and the heat extraction efficiency is obviously improved by increasing the action area of heat extraction. Because the treatment cost is low, the treatment condition is mild, the yield of the treated chlorella polysaccharide can be improved by 10-40% compared with the conventional hot water reflux, and the method has good industrial application prospect.
2. Through high-pressure blasting, that is, firstly, a very high pressure is applied to the material, then the pressure is released instantly, so that the purpose of blasting the material is achieved, and through the pretreatment of the material, on one hand, the structure of the fiber can be changed, the high extraction efficiency of heat extraction is realized, on the other hand, the decomposition of pectic substance, hemicellulose and lignin can be promoted, and the extraction rate of the green alga polysaccharide is improved without damaging the molecular structure of the polysaccharide.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings required to be used in the description of the embodiments will be briefly described below, and it is obvious that the drawings in the description below are only some embodiments of the present invention, and it is obvious for those skilled in the art that other drawings can be obtained based on the drawings without creative efforts.
FIG. 1 is a process flow diagram of the present invention;
FIG. 2 is a graph showing the effect of high pressure blasting reaction at different pressures on the extraction yield of Chlorella polysaccharide;
FIG. 3 is a graph showing the effect of different extraction temperatures on the extraction yield of Chlorella polysaccharide in the present invention;
FIG. 4 is a graph of heat extraction, high pressure blasting pretreatment combined with heat extraction of Chlorella polysaccharide in accordance with the present invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, preferred embodiments of the present invention will be described in detail below with reference to the accompanying drawings to facilitate understanding of the skilled person.
Example 1
Removing impurities from green algae, cleaning, drying, pulverizing, and sieving with 100 mesh sieve; taking the powder with 0.2% (W/V) K 2 CO 3 Preparing 3% (W/V) suspension from the solution, performing thermal reaction at 120 ℃ for 20min, and naturally cooling to normal temperature; carrying out a plurality of groups of high-pressure blasting reactions on the cooled suspension; the blasting pressures are respectively 40MPa, 60MPa, 80MPa and 100MPa; carrying out vacuum filtration on the brown viscous slurry liquid subjected to high-pressure blasting treatment to realize liquid-solid separation, and respectively collecting solid-phase and liquid-phase samples; washing the solid phase sample with distilled water for multiple times, inserting a pH meter into the distilled water during washing to detect the pH value until the pH value of the distilled water is 6-7, drying at 80 ℃ until the quality is unchanged, and crushing and sieving with a 100-mesh sieve; degreasing the sieved solid powder by using petroleum ether, wherein the solid-liquid ratio is 1g:30mL, and extracting by hot water reflux at 60 ℃ for 120min; vacuum filtering the extractive solution, concentrating the filtrate under reduced pressure, precipitating polysaccharide with anhydrous ethanol,centrifuging to obtain precipitate as Chlorella polysaccharide.
As shown in FIG. 2, the result showed that the yield of polysaccharide was highest (30.2%) at a burst pressure of 80MPa, after which the extraction rate began to decrease due to the destruction of the green algae fibers after burst caused by excessive pressure.
Example 2
(1) Removing impurities from green algae, cleaning, drying, pulverizing, and sieving with 100 mesh sieve; (2) Taking the powder with 0.2% (W/V) K 2 CO 3 Preparing 3% (W/V) suspension from the solution, performing thermal reaction at 120 ℃ for 20min, and naturally cooling to normal temperature; (3) carrying out high-pressure blasting reaction on the cooled suspension; the bursting pressure is 80MPa; (4) And (3) carrying out vacuum filtration on the brown viscous slurry liquid subjected to high-pressure blasting, carrying out liquid-solid separation, and respectively collecting a solid phase sample and a liquid phase sample. (5) Washing the solid phase sample with distilled water for multiple times, inserting a pH meter into the distilled water during washing to detect the pH value until the pH value of the distilled water is 6-7, drying at 80 ℃ until the quality is unchanged, and crushing and sieving with a 100-mesh sieve. (6) Degreasing the sieved solid powder by using petroleum ether, wherein the solid-liquid ratio is 1g:30mL, and then carrying out a plurality of groups of hot water reflux extraction experiments at different temperatures, wherein the temperatures are respectively 40 ℃, 60 ℃, 80 ℃ and 100 ℃, and the time is 120min; (7) Vacuum filtering the extractive solution, concentrating the filtrate under reduced pressure, precipitating polysaccharide with anhydrous ethanol, and centrifuging to obtain precipitate as Chlorella polysaccharide.
As shown in FIG. 3, the results showed that the polysaccharide yield was highest (30.2%) at a burst pressure of 60 ℃.
Comparative example 1
(1) Removing impurities from green algae, cleaning, drying, pulverizing, and sieving with 100 mesh sieve; (2) Taking the powder with 0.2% (W/V) K 2 CO 3 Preparing 3% (W/V) suspension from the solution, performing thermal reaction at 120 ℃ for 20min, and naturally cooling to normal temperature; (3) carrying out high-pressure blasting reaction on the cooled suspension; and (4) carrying out vacuum filtration on the brown viscous slurry liquid subjected to high-pressure blasting treatment at the blasting pressure of 80MPa, carrying out liquid-solid separation, and respectively collecting solid-phase and liquid-phase samples.
Comparative example 2
(1) Removing impurities from green algae, cleaning, drying, pulverizing, and sieving with 100 mesh sieve; (2) Defatting the sieved solid powder with petroleum ether, and performing reflux extraction with hot water, wherein the solid-liquid ratio is 1g:30mL, 60 ℃ and 120min; (3) Vacuum filtering the extractive solution, concentrating the filtrate under reduced pressure, precipitating polysaccharide with anhydrous ethanol, and centrifuging to obtain precipitate as Chlorella polysaccharide.
As shown in fig. 4, the results showed that the maximum extraction rate of polysaccharide by high pressure blasting pretreatment combined with heat extraction was 30.2%, which is 15.9% higher than 14.3% without high pressure blasting pretreatment.
Finally, it is noted that the above-mentioned preferred embodiments illustrate rather than limit the invention, and that, while the invention has been described in detail with reference to the foregoing preferred embodiments, it will be understood by those skilled in the art that various changes in form and detail may be made therein without departing from the scope of the invention as defined by the appended claims; the size of the attached drawing is irrelevant to a concrete object, and the size of the object can be changed at will.
Claims (5)
1. A high-pressure blasting-based extraction process of green alga polysaccharide is characterized by comprising the following steps: the method specifically comprises the following steps of,
s1: removing impurities from green algae, cleaning, drying, pulverizing, and sieving with 100 mesh sieve;
s2: taking the sieved powder, adding 0.2% of K 2 CO 3 Preparing solution into suspension of 3% W/V, thermally reacting at 120 deg.C for 20min, and naturally cooling to room temperature to obtain dark green suspension;
s3: and (3) carrying out high-pressure blasting reaction on the cooled suspension: pressurizing to 80MPa, and quickly releasing pressure;
s4: carrying out vacuum filtration on the dark green viscous pasty liquid subjected to high-pressure blasting treatment to realize liquid-solid separation, and respectively collecting a solid-phase sample and a liquid-phase sample;
s5: washing the solid phase sample for multiple times by using distilled water until the pH value of the washed distilled water is 6-7, then placing the solid phase sample in an environment of 80 ℃ for drying until the quality is unchanged, and then crushing the solid phase sample and sieving the crushed solid phase sample by using a 100-mesh sieve;
s6, degreasing the sieved solid powder by using petroleum ether, wherein the solid-liquid ratio is 1g: 20-50 mL, and then carrying out thermal extraction at 50-80 ℃ for 120min;
s7, vacuum filtering an extracting solution obtained by refluxing during hot extraction, concentrating the filtrate under reduced pressure, adding absolute ethyl alcohol to precipitate polysaccharide, and centrifuging to obtain a precipitate which is green alga polysaccharide;
s8: concentrating the liquid phase sample under reduced pressure, adding anhydrous ethanol to precipitate polysaccharide, and centrifuging to obtain precipitate as Chlorella polysaccharide.
2. The high pressure explosion-based extraction process of green alga polysaccharides as claimed in claim 1, wherein: in step S1, the selected green algae is blue algae or diatom.
3. The method for extracting green alga polysaccharide based on high pressure blasting as claimed in claim 1 or 2, wherein: and step S3, putting the suspension into a high-pressure homogenizer for high-pressure blasting reaction, wherein the flow is 10L/h, the blasting pressure is 80MPa, and the pressure relief time is not more than 5S.
4. The method for extracting chlorella polysaccharide based on high pressure blasting as claimed in claim 3, wherein the method comprises the following steps: in step S6, the solid-to-liquid ratio of the solid powder to the petroleum ether is 1g:40mL; the heat extraction temperature is 60 deg.C, and the time is 90min.
5. The method for extracting chlorella polysaccharide based on high pressure blasting as claimed in claim 4, wherein the method comprises the following steps: in step S7, the filtrate is decompressed and concentrated to 1/20 of the original extracting solution, the centrifugal rotating speed is 6000r/min, and the centrifugal time is 10min.
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102633894A (en) * | 2012-04-16 | 2012-08-15 | 中国科学院宁波材料技术与工程研究所 | Method for preparing high-concentration large-sized seaweed biomass solution and polysaccharide extract |
| CN104195198A (en) * | 2014-09-01 | 2014-12-10 | 石河子大学 | Method for extracting polysaccharide from chlorella |
| CN105646724A (en) * | 2014-12-03 | 2016-06-08 | 中国科学院大连化学物理研究所 | Method for extraction preparation of spirulina platensis soluble polysaccharide |
| CN105707072A (en) * | 2014-12-03 | 2016-06-29 | 中国科学院大连化学物理研究所 | Spirulina polysaccharide and application thereof |
| CN108003256A (en) * | 2017-12-25 | 2018-05-08 | 大连深蓝肽科技研发有限公司 | A kind of preparation method of high sulfate group algal polysaccharide |
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- 2022-07-04 CN CN202210785899.7A patent/CN115197337A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102633894A (en) * | 2012-04-16 | 2012-08-15 | 中国科学院宁波材料技术与工程研究所 | Method for preparing high-concentration large-sized seaweed biomass solution and polysaccharide extract |
| CN104195198A (en) * | 2014-09-01 | 2014-12-10 | 石河子大学 | Method for extracting polysaccharide from chlorella |
| CN105646724A (en) * | 2014-12-03 | 2016-06-08 | 中国科学院大连化学物理研究所 | Method for extraction preparation of spirulina platensis soluble polysaccharide |
| CN105707072A (en) * | 2014-12-03 | 2016-06-29 | 中国科学院大连化学物理研究所 | Spirulina polysaccharide and application thereof |
| CN108003256A (en) * | 2017-12-25 | 2018-05-08 | 大连深蓝肽科技研发有限公司 | A kind of preparation method of high sulfate group algal polysaccharide |
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Application publication date: 20221018 |