CN112979838A - Algal polysaccharide extract and preparation method and application thereof - Google Patents
Algal polysaccharide extract and preparation method and application thereof Download PDFInfo
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Abstract
The invention discloses a seaweed polysaccharide extract, application and a preparation method thereof. Wherein the algal polysaccharide extract is extracted from a composition of green algae and brown algae. In addition, the invention also discloses a preparation method of the algal polysaccharide extract, which comprises the following steps: step a: weighing green algae and brown algae according to a dry weight ratio, mixing, crushing, sieving the crushed materials, then carrying out ultrasonic extraction by adopting a calcium chloride aqueous solution, filtering the extracted solution, and collecting the filtrate; step b: adding polyamide and resin into the filtrate collected in the step a, stirring for a period of time, filtering, and collecting the filtrate; step c: and c, concentrating the filtrate collected in the step b to 1/5-1/8 of the original volume, filtering, adding ethanol into the filtrate, standing for 4-6 hours at 4-8 ℃, collecting solids, and drying to obtain the compound. The algal polysaccharide extract has a remarkable synergistic moisturizing effect, can effectively promote the repair of skin barriers, and can be used for developing moisturizing repair products.
Description
Technical Field
The invention belongs to the technical field of natural product extraction, and particularly relates to a seaweed extract, and a preparation method and application thereof.
Background
With the increase of age and the deterioration of external environment, the skin moisturizing function is reduced, and further, the collagen is dehydrated and hardened, and a series of problems of skin chapping, wrinkling, skin barrier damage and the like are caused. At present, hyaluronic acid is a well-known relatively ideal natural moisturizing factor, but hyaluronic acid is derived from animal tissues or genetic engineering fermentation, is different from pure natural hyaluronic acid derived from plants, has relatively single function, is mainly moisturizing and lubricating, and cannot repair damaged skin barriers. The plant-derived moisturizing factors have generally insufficient moisturizing effect.
Based on this, it is desired to obtain a natural moisturizing product which is simple in process, suitable for industrial production, includes several algae, has a synergistic moisturizing effect, and thus, has a better moisturizing effect than the components taken alone.
Disclosure of Invention
In order to solve the technical problems, the invention searches polysaccharide compositions with moisturizing and repairing effects from seaweeds. The seaweed is suitable for living environment with high salt and strong illumination, and generates a large amount of protective polysaccharide with various structures in the growth process so as to keep cell moisture and reduce cell damage. The algal polysaccharide composition provided by the invention has a synergistic interaction effect among the components in the aspect of moisturizing, and the moisturizing effect is obviously superior to that of single algal polysaccharide. The algal polysaccharide composition provided by the invention can also effectively promote the repair of skin barriers.
Aiming at the defects of the prior art, the invention provides a seaweed polysaccharide extract, application and a preparation method thereof, which are realized by the following technical scheme:
in a first aspect, the present invention provides a algal polysaccharide extract, which is extracted from a composition of green algae and brown algae.
Preferably, the green algae is Ulva (Ulva lactuca).
Preferably, the brown algae comprises Fucus vesiculosus (Fucus vesiculosus).
Preferably, the dry weight ratio of green algae to fucus is: 1: 5 to 80.
Preferably, the brown algae further comprises other brown algae selected from the following group: at least one of Zostera marina (Sargassum pallidum), Hizikia fusiforme (Hizikia fusiforme), and Undaria pinnatifida (Undaria pinnatida).
Preferably, the dry weight ratio of the green algae to other brown algae is 1: 0.2-16.
In a second aspect, the present invention provides a preparation method of the algal polysaccharide extract, wherein the preparation method comprises the following steps:
step a: weighing green algae and brown algae according to a dry weight ratio, mixing, crushing, sieving the crushed materials, then carrying out ultrasonic extraction by adopting a calcium chloride aqueous solution, filtering the extracted solution, and collecting the filtrate;
step b: adding polyamide and resin into the filtrate collected in the step a, stirring for a period of time, filtering, and collecting the filtrate;
step c: and c, concentrating the filtrate collected in the step b to 1/5-1/8 of the original volume, filtering, adding ethanol into the filtrate, standing for 4-6 hours at 4-8 ℃, collecting solids, and drying to obtain the compound.
Preferably, in the step a, the sieving is performed by using a 10-mesh sieve, and the ultrasonic extraction is performed under the process conditions that the power of the ultrasonic extraction is 250-600W, the extraction time is 20-30 minutes, and the extraction is performed for 2 times.
Preferably, in the step b, the adding amount of the polyamide is 0.5-10% of the total mass of the filtrate, the adding amount of the resin is 0.5-10% of the total mass of the filtrate, and the stirring time is 1 h.
In a preferable embodiment, in the step a, the weight ratio of the algae powder after passing through the 10-mesh sieve to the calcium chloride aqueous solution is 1:6 to 1:20, preferably 1:10 to 1: 15.
In a preferable embodiment, in the step a, the mass percentage of calcium chloride is 0.1-5%, and more preferably, the mass percentage of calcium chloride is 0.5-2%.
As a preferred technical solution, in the step b, the resin is selected from cation exchange resin, anion exchange resin and composite ion exchange resin, more preferably, the resin is composite ion exchange resin, and further preferably, the resin is snake cage resin;
as a preferable technical scheme, in the step b, the adding amount of the polyamide and/or the resin is 0.5-10% of the weight of the filtrate, and preferably the adding amount of the polyamide and/or the resin is 1-5% of the weight of the filtrate;
as a preferred technical scheme, in the step c, after the ethanol is added, the final volume fraction of the ethanol is 60-80%.
In a third aspect, the invention provides an application of the algal polysaccharide extract, and the algal polysaccharide extract is used in cosmetics for moisturizing and repairing.
Compared with the prior art, the algal polysaccharide extract, the application and the preparation method thereof have the following advantages and beneficial effects:
the seaweed polysaccharide extract provided by the invention has obvious synergistic moisturizing effect on each component due to the diversity of the structures of the polysaccharides of the green algae and the brown algae.
This is because: in the present case, green algae are used because the green algae contain green algae polysaccharides that are acidic polysaccharides and contain uronic acid groups in the molecule, as does hyaluronic acid. The brown algae is adopted because the brown algae contains fucoidan which is neutral polysaccharide, mainly fucoidan sulfate, and different brown algae, and monosaccharide composition, molecular weight and branching degree of the contained fucoidan sulfate are not completely the same.
In addition, the inventor of the present invention finds, through research, that the algal polysaccharide extract of the present invention has a good synergistic effect of moisturizing, and may have the following two reasons:
firstly, the polysaccharide extracts in the scheme have different molecular weights and branching degrees of various sugars. The small molecular weight polysaccharide is filled into the branched structures of the large molecular weight polysaccharide and the sugar chain to form a compact network structure, and has an ultra-strong water locking function.
Secondly, the acidic polysaccharide provided by the green algae in the scheme contains carboxyl, the capability of forming hydrogen bonds is stronger than that of neutral polysaccharide, and the strong hydrogen bond has stronger water absorption capability on one hand and can make the compact reticular structure firmer and keep the super-strong water locking function for a long time on the other hand.
Drawings
Other features, objects and advantages of the invention will become more apparent upon reading of the detailed description of non-limiting embodiments with reference to the following drawings:
FIG. 1 shows the results of the moisture retention test of samples prepared in examples 1 to 4 of the present invention and comparative examples 1 and 2;
FIG. 2 shows the results of the test for promoting expression of filaggrin in samples prepared in examples 1 and 2 of the present invention.
Detailed Description
The present invention will be described in detail with reference to specific examples. The following examples will assist those skilled in the art in further understanding the invention, but are not intended to limit the invention in any way. It should be noted that it would be obvious to those skilled in the art that various changes and modifications can be made without departing from the spirit of the invention. All falling within the scope of the present invention.
Example 1
Example 1 provides a method for preparing a algal polysaccharide extract, in this example, the weight ratio of ulva, fucus and other brown algae is 1:16.7:2.3, which specifically includes the following steps:
(1) taking 10g of dried ulva, 167g of sea oak, 11g of kelp, 6g of sargassum fusiforme and wakame seaweed respectively, mixing and powdering, sieving by a 10-mesh sieve, and ultrasonically extracting the sieved alga body powder for 2 times, 20 minutes each time (the power of ultrasonic extraction is 400W) by using 2.0kg of calcium chloride aqueous solution with the mass percent of 1%. Mixing the two extractive solutions, and filtering with 5 μm polypropylene membrane to obtain 2.9kg filtrate;
(2) adding 50g of polyamide and 50g of snake cage resin into the filtrate obtained in the step (1), stirring for 1 hour at room temperature, and filtering by using a 0.8-micron polypropylene membrane to obtain 2.6kg of filtrate;
(3) concentrating the filtrate of step (2) at 55 deg.C under reduced pressure to about 450ml, filtering with 0.8 μm polypropylene membrane, collecting filtrate, adding ethanol into the filtrate to make ethanol final concentration (volume percentage) 75%, standing at 4 deg.C for 5 hr, centrifuging, collecting solid, and drying to obtain polysaccharide extract 4.3 g.
Example 2
Example 2 provides a method for preparing a algal polysaccharide extract, in this example, the weight ratio of ulva, fucus and other brown algae is 1:80:15, which specifically includes the following steps:
(1) taking 2g of dried ulva, 160g of Fucus vesiculosus, 10g of kelp, 10g of Cyrtymenia Sparsa and 10g of Undaria pinnatifida, mixing, pulverizing, sieving with a 10-mesh sieve, and ultrasonically extracting the sieved alga body powder with 2kg of calcium chloride aqueous solution with the mass percent of 1% for 2 times, wherein the ultrasonic extraction power is 400W each time. Mixing the two extractive solutions, and filtering with 5 μm polypropylene membrane to obtain 3.0kg filtrate;
(2) adding 60g of polyamide and 60g of snake cage resin into the filtrate obtained in the step (1), stirring for 1 hour at room temperature, and filtering by using a 0.8-micron polypropylene membrane to obtain 2.5kg of filtrate;
(3) concentrating the filtrate of step (2) at 55 deg.C under reduced pressure to about 400ml, filtering with 0.8 μm polypropylene membrane, collecting filtrate, adding ethanol into the filtrate to make ethanol final concentration (volume percentage) 75%, standing at 4 deg.C for 5 hr, centrifuging, collecting solid, and drying to obtain polysaccharide extract 4.0 g.
Example 3
Example 3 provides a method for preparing a algal polysaccharide extract, the weight ratio of ulva, fucus and other brown algae is 1:167: 2.3. The method specifically comprises the following steps:
(1) taking 1g of dried ulva, 167g of sea oak, 1.1g of kelp, 0.6g of sargassum fusiforme and 0.6g of undaria pinnatifida, mixing, pulverizing, sieving by a 10-mesh sieve, and ultrasonically extracting algae powder obtained by sieving by 1.9kg of calcium chloride aqueous solution with the mass percent of 1% for 2 times, wherein the ultrasonic extraction power is 400W each time. Mixing the two extractive solutions, and filtering with 5 μm polypropylene membrane to obtain 3.0kg filtrate;
(2) adding 50g of polyamide and 50g of snake cage resin into the filtrate obtained in the step (1), stirring for 1 hour at room temperature, and filtering by using a 0.8-micron polypropylene membrane to obtain 2.7kg of filtrate;
(3) concentrating the filtrate of step (2) at 55 deg.C under reduced pressure to about 450ml, filtering with 0.8 μm polypropylene membrane, collecting filtrate, adding ethanol into the filtrate to make ethanol final concentration (volume percentage) 75%, standing at 4 deg.C for 5 hr, centrifuging, collecting solid, and drying to obtain polysaccharide extract 4.1 g.
Example 4
Example 4 provides a method for preparing a algal polysaccharide extract, the weight ratio of ulva, fucus and other brown algae is 1:1.67: 2.3. The method specifically comprises the following steps:
(1) taking 50g of dried ulva, 83.5g of Fucus vesiculosus, 49g of kelp, 33g of Cyrtymenia Sparsa and 33g of Undaria pinnatifida, mixing, pulverizing into powder, sieving with a 10-mesh sieve, and ultrasonically extracting the sieved alga body powder with 2.5kg of calcium chloride aqueous solution with the mass percent of 1% for 2 times, wherein the ultrasonic extraction power is 400W each time. Mixing the two extractive solutions, and filtering with 5 μm polypropylene membrane to obtain filtrate 3.9 kg;
(2) adding 50g of polyamide and 50g of snake cage resin into the filtrate obtained in the step (1), stirring for 1 hour at room temperature, and filtering by using a 0.8-micron polypropylene membrane to obtain 3.7kg of filtrate;
(3) concentrating the filtrate of step (2) at 55 deg.C under reduced pressure to about 600ml, filtering with 0.8 μm polypropylene membrane, collecting filtrate, adding ethanol to the filtrate to make ethanol concentration (volume percentage) 75%, standing at 4 deg.C for 5 hr, centrifuging, collecting solid, and drying to obtain polysaccharide extract 5.0 g.
Comparative example 1
Comparative example 1 provides a preparation method of algal polysaccharide extract, comparative example 1 uses only brown algae without green algae, and the weight ratio of fucus vesiculosus to other brown algae is 16.7:2.3, and specifically comprises the following steps:
(1) mixing 167g of dried Fucus vesiculosus, 11g of kelp, 6g of Cyrtymenia Sparsa and Undaria pinnatifida, pulverizing, sieving with a 10-mesh sieve, and ultrasonically extracting the sieved alga powder with 1.9kg of calcium chloride aqueous solution with the mass percent of 1% for 2 times, 20 minutes each time (the power of ultrasonic extraction is 400W). Mixing the two extractive solutions, and filtering with 5 μm polypropylene membrane to obtain 2.8kg filtrate;
(2) adding 50g of polyamide and 50g of snake cage resin into the filtrate obtained in the step (1), stirring for 1 hour at room temperature, and filtering by using a 0.8-micron polypropylene membrane to obtain 2.6kg of filtrate;
(3) concentrating the filtrate of step (2) at 55 deg.C under reduced pressure to about 500ml, filtering with 0.8 μm polypropylene membrane, collecting filtrate, adding ethanol into the filtrate to make ethanol final concentration be 75%, standing at 4 deg.C for 5 hr, centrifuging, collecting solid, and drying to obtain polysaccharide extract 3.9 g.
Comparative example 2
Comparative example 2 provides a method for preparing algal polysaccharide extract, and comparative example 2 uses only green algae, and specifically comprises the following steps:
(1) taking 100g of dried ulva, mixing, pulverizing, sieving with a 10-mesh sieve, and ultrasonically extracting algae powder obtained by sieving with 1kg of calcium chloride aqueous solution with the mass percent of 1% for 2 times, wherein the ultrasonic extraction power is 400W each time. Mixing the two extractive solutions, and filtering with 5 μm polypropylene membrane to obtain 1.6kg filtrate;
(2) adding 30g of polyamide and 30g of snake cage resin into the filtrate obtained in the step (1), stirring for 1 hour at room temperature, and filtering by using a 0.8-micron polypropylene membrane to obtain 1.4kg of filtrate;
(3) concentrating the filtrate of step (2) at 55 deg.C under reduced pressure to about 200ml, filtering with 0.8 μm polypropylene membrane, collecting filtrate, adding ethanol into the filtrate to make ethanol final concentration be 75%, standing at 4 deg.C for 5 hr, centrifuging, collecting solid, and drying to obtain polysaccharide extract 2.6 g.
Evaluation of efficacy
1. Test for moisturizing Effect
The algal polysaccharide extracts prepared in examples 1-4 of the present invention and comparative examples 1 and 2 were tested for their moisturizing effect. 0.2% algal polysaccharide extract and 0.2% hyaluronic acid were applied to different areas of the inner forearm of 14 volunteers, respectively, and the Moisture content of the horny layer of the forearm skin was measured before application and 6 hours after application (CM 825 skin probe) and the change rate MMV% of the Moisture Measurement Value (Moisture Measurement Value) was calculated, blank control applied water.
The calculation formula of MMV% is
MMV％＝100％×(MMV6-MMV0)/MMV0
In the formula, MMV6The moisture content of the skin after 6 hours of sample application; MMV0The moisture content of the skin before the sample is smeared;
the test results are shown in fig. 1, and the larger the MMV% is, the better the moisturizing effect is. As can be seen from fig. 1, the effects of examples 1 and 2 are significantly better than those of comparative examples 1 and 2 and examples 3 and 4, which shows that the components of the algal polysaccharide extract are significantly better than those of comparative examples 1 and 2 with a single component, and each component has a significant synergistic moisturizing effect.
Particularly, when the dry weight ratio of ulva, fucus and other brown algae is 1: (50-80): (0.2 to 16), the synergistic moisturizing state is particularly remarkable.
2. Skin barrier repair test
Filaggrin (FLG) is an important molecule in the stratum corneum of human skin that connects keratin fibers, and is involved in the differentiation of epidermal cells and the formation of the skin barrier. The increased FLG expression level indicates that the skin barrier repair effect is enhanced.
Algal polysaccharide compositions prepared in examples 1 and 2 of the present invention were co-cultured with NHEK cells for 24 hours, and then the relative expression level of FLG mRNA was measured (algal polysaccharide composition concentration: 50. mu.g/ml). The ratio of the FLG expression level of the sample group to the FLG expression level of the blank control group is shown in FIG. 2, and the algal polysaccharide compositions provided in examples 1 and 2 of the present invention increase the FLG expression level by nearly one time, which indicates that the algal polysaccharide compositions provided by the present invention can promote the repair of skin barrier.
The foregoing examples are merely illustrative and serve to explain some of the features of the method of the present invention. The present invention is not limited to the above-described embodiments, which do not mean that the present invention must be practiced by the above-described embodiments. It should be understood by those skilled in the art that any modification of the present invention, equivalent substitutions of the raw materials of the product of the present invention, addition of auxiliary components, selection of specific modes, etc., are within the scope and disclosure of the present invention.
Claims (10)
1. An algal polysaccharide extract, which is characterized in that the algal polysaccharide extract is extracted from a composition of green algae and brown algae.
2. The algal polysaccharide extract of claim 1, wherein the green algae are ulva.
3. The algal polysaccharide extract of claim 1, wherein the brown algae comprises Fucus vesiculosus.
4. The algal polysaccharide extract of claim 3, wherein the dry weight ratio of green algae to fucus is: 1: 5 to 80.
5. The algal polysaccharide extract of claim 3, wherein the brown algae further comprises other brown algae selected from the group consisting of: at least one of kelp, sargassum fusiforme and wakame seaweed.
6. The algal polysaccharide extract of claim 5, wherein the dry weight ratio of the green algae to other brown algae is 1: 0.2-16.
7. A process for the preparation of algal polysaccharide extract according to any one of claims 1-6, wherein the process comprises the steps of:
step a: weighing green algae and brown algae according to a dry weight ratio, mixing, crushing, sieving the crushed materials, then carrying out ultrasonic extraction by adopting a calcium chloride aqueous solution, filtering the extracted solution, and collecting the filtrate;
step b: adding polyamide and resin into the filtrate collected in the step a, stirring for a period of time, filtering, and collecting the filtrate;
step c: and c, concentrating the filtrate collected in the step b to 1/5-1/8 of the original volume, filtering, adding ethanol into the filtrate, standing for 4-6 hours at 4-8 ℃, collecting solids, and drying to obtain the compound.
8. The method for preparing algal polysaccharide extract according to claim 7, wherein in the step a, the sieving is performed by 10 mesh, and the ultrasonic extraction is performed under the process conditions that the power of the ultrasonic extraction is 250-600W, the extraction time is 20-30 minutes, and the extraction is performed for 2 times.
9. The method for preparing algal polysaccharide extract according to claim 7, wherein in the step b, the amount of the polyamide added is 0.5% to 10% of the total mass of the filtrate, the amount of the resin added is 0.5% to 10% of the total mass of the filtrate, and the stirring time is 1 hour.
10. Use of the algal polysaccharide extract according to any one of claims 1-6, wherein the algal polysaccharide extract is used in a cosmetic for moisturizing repair.
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