CN112370465A - Sargassum fusiforme polysaccharide functionalized nano-selenium and preparation method and application thereof - Google Patents
Sargassum fusiforme polysaccharide functionalized nano-selenium and preparation method and application thereof Download PDFInfo
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Abstract
The invention discloses a sargassum fusiforme polysaccharide functionalized nano-selenium and a preparation method and application thereof. The preparation method of the sargassum fusiforme polysaccharide functionalized nano-selenium comprises the following steps: mixing the polysaccharide solution of Cyrtymenia Sparsa with sodium selenite by chemical reduction method, adding ascorbic acid solution, water bathing, dialyzing, and lyophilizing to obtain the final product. The invention takes sodium selenite as a selenium source, ascorbic acid as a reducing agent and Sargassum Fusiforme Polysaccharide (SFPS) as a modifier to prepare polysaccharide nano selenium complex (SFPS-SeNPs) with good stability and high solubility. The invention provides a new idea and a new development for extracting sargassum fusiforme polysaccharide and developing selenium supplement products. Compared with the original nano-selenium particles, the Sargassum fusiforme polysaccharide functionalized nano-selenium prepared by the invention has improved antioxidant activity, and the antioxidant activity of the Sargassum fusiforme polysaccharide is not reduced after the Sargassum fusiforme polysaccharide is compounded with the nano-selenium, so the Sargassum fusiforme polysaccharide functionalized nano-selenium is a polysaccharide nano-selenium compound with good stability and high solubility.
Description
Technical Field
The invention belongs to the technical field of nano-selenium preparation, and particularly relates to sargassum fusiforme polysaccharide functionalized nano-selenium and a preparation method and application thereof.
Background
Selenium is an essential trace element for the human body, and at the same time, it can help cells to resist oxidative damage and also plays an important role in various neurodegenerative diseases. In vivo, the main existing forms of selenium element are various selenoproteins, thereby playing important roles in redox regulation and control of various cells, detoxification and immune system protection. However, many of the beneficial physiological effects of selenium tend to be toxic depending on higher intake, limiting its use. The nano-selenium is in a simple substance selenium form with high efficiency and low toxicity, and has wide selection source and excellent biocompatibility. In reported methods for controlling nanoparticle growth, polysaccharides, proteins and/or lipids have been used as effective nanocarriers for SeNPs. More and more evidences show that the biological activity polysaccharide used as the modifier of the nano-selenium can obviously improve the stability, the biocompatibility and various biological activities of the nano-selenium. Therefore, the preparation of nano selenium with small particle size and high stability by using natural polysaccharide as a modifier has become a hot point of current research.
Cyrtymenia Sparsa belongs to Fucales of Phaeophyta, and has been distributed in peninsula, Fujian, and Guangdong shallow sea areas in Liaodong, and also has been grown in Korea in Japan. The sargassum fusiforme is rich in polysaccharide, food cellulose, various vitamins, minerals and trace elements, and has 18 important amino acids required by human body. The sargassum fusiforme polysaccharide is an acidic polysaccharide with various pharmacological activities, mainly comprises alginic acid and fucoidan, and has the content of 16-24% in dry sargassum fusiforme. Sargassum Fusiforme Polysaccharide (SFPS) is an effective and nontoxic natural compound as one of the main effective activities, and is a better choice as a nano selenium modifier.
Chinese patent CN111406948A discloses a method for preparing nano-selenium, which takes sodium selenite as a selenium source, ascorbic acid as a reducing agent and Grateloupia filicina polysaccharide as a modifier to prepare the nano-selenium with stable grain diameter of about 60nm and strong antioxidant activity; chinese patent CN109650349A discloses a preparation method of camellia plant polysaccharide functionalized nano-selenium, and discloses the enhancement effect of camellia plant polysaccharide on the functional characteristics of nano-selenium; at present, the preparation and activity research of the sargassum fusiforme polysaccharide as a modifier of nano selenium is not reported yet.
Disclosure of Invention
In order to overcome the defects in the prior art, the invention aims to provide the sargassum fusiforme polysaccharide functionalized nano-selenium and the preparation method and the application thereof.
The invention aims to provide sargassum fusiforme polysaccharide functionalized nano-selenium and a preparation method and application thereof, so as to solve the problems in the prior art.
The invention takes sargassum fusiforme polysaccharide as a modifier, prepares a polysaccharide solution with a certain concentration to be mixed with a sodium selenite solution, slowly adds an ascorbic acid solution to prepare a polysaccharide-nano selenium compound with high stability and good solubility by a chemical reduction method, and then applies the sargassum fusiforme polysaccharide nano selenium compound to an antioxidant drug.
The purpose of the invention is realized by at least one of the following technical solutions.
The invention provides a method for preparing sargassum fusiforme polysaccharide functionalized nano selenium (SFPS-SeNPs) by using the sargassum fusiforme polysaccharide, which comprises the following steps:
(1) uniformly mixing the sargassum fusiforme polysaccharide solution and the sodium selenite solution, slowly adding the ascorbic acid solution, uniformly stirring, heating to perform water bath reaction to obtain a reaction solution;
(2) and (2) dialyzing the reaction solution obtained in the step (1), and freeze-drying to obtain the sargassum fusiforme polysaccharide functionalized nano selenium (SFPS-SeNPs).
Further, the concentration of the sargassum fusiforme polysaccharide solution in the step (1) is 0.25-3 mg/mL;
further, the concentration of the sodium selenite solution in the step (1) is 0.01 mol/L;
further, the concentration of the ascorbic acid solution in the step (1) is 0.04 mol/L;
further, the volume ratio of the sargassum fusiforme polysaccharide solution, the sodium selenite solution and the ascorbic acid solution in the step (1) is 1:1: 1;
further, the temperature of the water bath reaction in the step (1) is 50 +/-5 ℃, and the time of the water bath reaction is 4 +/-0.5 h.
Preferably, the concentration of the sodium selenite solution in the step (1) is 0.01 mol/L.
Preferably, the concentration of the ascorbic acid solution in the step (1) is 0.04 mol/L.
Preferably, the volume ratio of the sargassum fusiforme polysaccharide solution, the sodium selenite solution and the ascorbic acid solution in the step (1) is 1:1: 1.
preferably, the temperature of the water bath reaction in the step (1) is 50 ℃, and the time of the water bath reaction is 4 hours.
Further, the dialysis treatment in the step (2) adopts a dialysis bag with the molecular weight cut-off of 3-4kD, the dialysis treatment time is 48-72h, and the dialysis treatment temperature is 4 ℃.
Preferably, the dialysis treatment of step (2) employs a dialysis bag with a molecular weight cut-off of 3kD, the dialysis treatment time is 48h, and the dialysis treatment temperature is 4 ℃.
The invention provides a sargassum fusiforme polysaccharide functionalized nano selenium (sargassum fusiforme polysaccharide-nano selenium compound) prepared by the preparation method. The Sargassum fusiforme polysaccharide functionalized nano-selenium has antioxidant activity.
The sargassum fusiforme polysaccharide functionalized nano-selenium provided by the invention can be applied to preparation of antioxidant and selenium supplement products.
Compared with the prior art, the invention has the following advantages and beneficial effects:
(1) according to the preparation method of the sargassum fusiforme polysaccharide functionalized nano-selenium provided by the invention, sodium selenite and ascorbic acid are directly used as raw materials, sargassum fusiforme polysaccharide is used as a surface modifier, the preparation process is simple and feasible, the product system is simple, the particle size of the prepared nano-selenium particles is small, the dispersion degree is high, the particle size does not change obviously within one month of storage at 4 ℃, and the energy spectrum analysis shows that the content of selenium atoms in the prepared polysaccharide-nano-selenium is 11.88%;
(2) compared with the original nano-selenium particles, the Sargassum fusiforme polysaccharide functionalized nano-selenium prepared by the invention has improved antioxidant activity, and the antioxidant activity of the Sargassum fusiforme polysaccharide is not reduced after the Sargassum fusiforme polysaccharide is compounded with the nano-selenium, so the Sargassum fusiforme polysaccharide functionalized nano-selenium is a polysaccharide nano-selenium compound with good stability and high solubility.
Drawings
FIG. 1a is a line graph showing the yield of crude polysaccharide versus the feed-to-liquid ratio;
FIG. 1b is a plot of crude polysaccharide yield versus water bath time;
FIG. 1c is a plot of crude polysaccharide yield versus ultrasonic power;
FIG. 1d is a graph of crude polysaccharide yield versus ultrasound time line;
FIG. 2 is a graph of particle size of Hizikia fusiforme polysaccharide modified nano-selenium solution with different concentrations;
FIG. 3a is a transmission electron microscope image of the nano-selenium solution;
FIG. 3b is the transmission electron microscope image of the polysaccharide-nano selenium solution of Cyrtymenia Sparsa;
FIG. 4 is a surface element energy spectrum analysis diagram of Hizikia fusiforme polysaccharide-nano selenium;
FIG. 5 is a graph of the ultraviolet absorption spectrum of nano-selenium and Hizikia fusiforme polysaccharide-nano-selenium;
FIG. 6a is a graph comparing the DPPH radical scavenging ability of different concentrations of nano-selenium, Hizikia fusiforme polysaccharide and Hizikia fusiforme polysaccharide-nano selenium solution;
FIG. 6b is a graph comparing the hydroxyl radical scavenging ability of different concentrations of nano-selenium, Hizikia fusiforme polysaccharide and Hizikia fusiforme polysaccharide-nano selenium solution;
FIG. 6c is a graph comparing the ABTS free radical scavenging ability of different concentrations of nano-selenium, Hizikia fusiforme polysaccharide and Hizikia fusiforme polysaccharide-nano selenium solution.
Detailed Description
The following description of the embodiments of the present invention is provided in connection with the accompanying drawings and examples, but the invention is not limited thereto. It is noted that the processes described below, if not specifically described in detail, are all realizable or understandable by those skilled in the art with reference to the prior art. The reagents or apparatus used are not indicated to the manufacturer, and are considered to be conventional products available by commercial purchase.
Example 1 optimization of extraction Process of Hizikia fusiforme polysaccharide
1. Single factor experiment
In the experiment of extracting sargassum fusiforme polysaccharide by ultrasonic-assisted hot water, the method comprises the following steps:
(1) pulverizing dried Cyrtymenia Sparsa powder with a pulverizer, sieving with 40 mesh sieve, refluxing with 95 vol% ethanol at 70 deg.C for 3 hr (m/v ═ 1:4), decolorizing, vacuum filtering, collecting residue, and drying at 50 deg.C for 12 hr to obtain decolorized Cyrtymenia Sparsa.
(2) Preparing the decolorized sargassum fusiforme solution with distilled water according to a feed-liquid ratio of 1:20-60g/mL, setting ultrasonic parameters (ultrasonic power of 200-.
Extraction conditions are as follows: the ratio of the material to the liquid is 1:20-60, the water bath time is 60-180min, the ultrasonic power is 200-600W, and the ultrasonic time is 10-30 min.
(3) And (3) carrying out rotary evaporation and concentration on the sargassum fusiforme polysaccharide extracting solution obtained in the step (2) at 55 ℃ to 1/4 of the original volume, adding absolute ethyl alcohol of which the volume is 4 times that of the concentrated extracting solution, precipitating in a refrigerator at 4 ℃ for 12-24h, centrifuging at 8000r for 20min to obtain sargassum fusiforme crude polysaccharide, adding water for redissolving, and freeze-drying and weighing.
In the formula: w is the weight (g) of the crude polysaccharide after freeze-drying in the step (3); w0 is the weight of decolorized Cyrtymenia Sparsa powder
(4) And removing protein and desalting by sevage method, dialyzing, and freeze-drying for storage.
The extraction rate of the sargassum fusiforme polysaccharide can be influenced by various factors, in order to explore the mutual relation, the feed-liquid ratio, the water bath time, the ultrasonic power and the ultrasonic time are set to be four factors, one factor is changed, and other factors are unchanged, so that a single-factor test is carried out.
1.1 feed-to-liquid ratio
In order to explore the influence of the feed liquid ratio on the extraction rate of the sargassum fusiforme polysaccharide, the invention sets the feed liquid ratio to be 1:20, 1:30, 1:40, 1:50 and 1:60, the ultrasonic power to be 300W, the ultrasonic time to be 20min and the water bath time to be 20min, extracts the polysaccharide under the conditions according to the method, and detects the yield of the crude polysaccharide under different conditions.
As shown in FIG. 1a, the extraction rate of sargassum fusiforme polysaccharide is not continuously increased along with the increase of the feed-to-liquid ratio, the extraction rate of sargassum fusiforme polysaccharide reaches up to 23.2% when the feed-to-liquid ratio is 1:40, the feed-to-liquid ratio is continuously increased, and the polysaccharide yield is not obviously changed. The result shows that the increase of the water amount can provide more dissolving space for the polysaccharide, so that the yield of the polysaccharide is improved, but the polysaccharide content is gradually saturated and the yield tends to be flat along with the increase of the feed-liquid ratio. In addition, the subsequent workload and cost are increased by increasing the ratio of the material to the liquid, so that the range of the ratio of the material to the liquid is selected to be about 1: 40.
1.2 Water bath time
In order to explore the influence of ultrasonic power on the extraction rate of the sargassum fusiforme polysaccharide, the invention sets water bath time for 60min, 90min, 120min, 150min and 180min, the feed-liquid ratio is 1:40, the ultrasonic power is 400W, and the ultrasonic time is 20min, extracts the sargassum fusiforme polysaccharide under the condition and measures the polysaccharide yield.
As shown in FIG. 1b, the yield of sargassum fusiforme polysaccharide increased from 18.8% to 22.4% during the water bath time increased from 60min to 120min, and then the polysaccharide yield decreased to about 20.5% instead as the water bath time increased. The result shows that the extraction rate of the polysaccharide can be improved by increasing the temperature, but the structure of the polysaccharide can be changed and even the polysaccharide is inactivated by overhigh temperature, so the water bath time is selected to be about 120 min.
1.3 ultrasonic power
In order to explore the influence of the ultrasonic power on the extraction rate of the polysaccharide of the sargassum fusiforme, the ultrasonic power is set as follows: 200W, 300W, 400W, 500W and 600W, the material-liquid ratio is 1:40, the ultrasonic time is 20min, the water bath time is 120min, the polysaccharide is extracted by the same method, and the crude polysaccharide yield is measured.
As shown in FIG. 1c, the yield of polysaccharide was at most 23.8% when the ultrasonic power was increased to 300W, but the yield of polysaccharide was drastically decreased when the ultrasonic power was increased, and the yield of polysaccharide was already decreased to about 16% when the ultrasonic power was increased to 500W. The results show that ultrasound of appropriate intensity contributes to the disruption of the cell walls of sargassum fusiforme to release more polysaccharides, but too high ultrasound intensity can destroy the structure and activity of polysaccharides, which may also be related to the formation of ultrasound shielding effect. Therefore, the ultrasonic intensity is selected to be about 300W.
1.4 ultrasound time
In order to explore the influence of ultrasonic time on the extraction rate of the sargassum fusiforme polysaccharide, the ultrasonic time is set to be 10min, 15min, 20min, 25min and 30min, the feed-liquid ratio is 1:40(g/mL), the ultrasonic power is 400W, and the water bath time is 120 min.
The result is shown in fig. 1d, in the process of increasing the ultrasound time from 10min to 20min, the hizikia fusiforme polysaccharide yield is remarkably increased from 17.8% to 23%, the ultrasound time is continuously increased to cause the remarkable reduction of the polysaccharide yield, and the trend is similar to the influence trend of the ultrasound power on the polysaccharide yield. The result shows that proper ultrasonic time is helpful for the release and dissolution of the sargassum fusiforme polysaccharide, but the cavitation shielding effect generated by long-time ultrasonic reduces the yield of the polysaccharide, so the ultrasonic time is selected to be about 20 min.
2. Response surface optimization experiment
On the basis of a single-factor experiment result, designing a response surface optimization experiment by using Design-Expert software: a total of 29 experiments are designed according to a scheme of 4 factors and 3 levels, the experiments are carried out one by one according to the above sargassum fusiforme polysaccharide extraction method, the crude polysaccharide yield of each group of experiments is recorded and analyzed, and the design and the result are shown in Table 1.
TABLE 1
Significance and analysis of variance were performed on the basis of the experimental results of table 1, and the results are shown in table 2:
TABLE 2
As can be seen from Table 2, the linear parameters (A, B, C), the quadratic parameters (A2, D2) and the interactive parameters (AC) significantly affect the SFPS yield, the P values of the model are very significant, indicating that the fitness of the model is high, while the absence of the fit values indicates that the fitness is not significant relative to pure errors. The predicted optimal extraction conditions were: the ratio of the feed to the liquid is 1:50, the ultrasonic power is 20OW, the ultrasonic time is 15min, the water bath time is 130min, and the yield theoretical value of the polysaccharide under the condition is 26%.
In order to check whether the calculated optimal extraction conditions are the same as the real conditions, an approximate verification experiment is performed. The experiment is carried out for 3 times in parallel according to the optimal extraction condition of the sargassum fusiforme polysaccharide, the average yield of the obtained sargassum fusiforme polysaccharide is 25.8 percent, the error from a theoretical value is small, the repeatability is good, and the result is reliable.
Example 2 preparation of Hizikia fusiforme polysaccharide functionalized nano-selenium (SFPS-SeNP)
Adopting a chemical reduction method to prepare the sargassum fusiforme polysaccharide-nano selenium. Mixing hizikia fusiforme polysaccharide solution (1mg/mL) with the concentration of 0.25,0.5,1,2,3,4mg/mL and 0.01mol/L sodium selenite solution in equal volume, uniformly mixing for about 20min under the action of magnetic stirring, then adding ascorbic acid solution with equal volume of 0.04mol/L into the mixed solution, and reacting for 4h under the condition of magnetic stirring at 50 ℃ until orange red solution with stable color is formed. Transferring the reaction solution into a dialysis bag with molecular weight cutoff of 3kD, dialyzing in a refrigerator at 4 ℃ for 48h, and freeze-drying to obtain Sargassum fusiforme polysaccharide functionalized nano selenium compound powder, and storing in a dryer. The same operation as above, the Sargassum fusiforme solution is changed into deionized water solution with the same volume to prepare nano-selenium solution, and the nano-selenium solution is dialyzed and freeze-dried to obtain nano-selenium powder which is stored in a dryer. And respectively adopting a laser particle size analyzer, a Transmission Electron Microscope (TEM), an energy spectrum analysis chart and an ultraviolet absorption spectrum to characterize the nano selenium.
In this example, the influence of different concentrations of hizikia fusiforme polysaccharide in the reaction system on the particle size of the nano-selenium particles in the reaction system is examined, and the results are shown in fig. 2, and the hizikia fusiforme polysaccharide solutions of 0.25,0.5,1,2,3 and 4mg/mL are respectively selected as the modifier of nano-selenium in the present invention. When the concentration of the sargassum fusiforme polysaccharide solution is 0.25-1mg/mL, the particle size of the nano selenium is gradually reduced; when the concentration of the sargassum fusiforme polysaccharide solution exceeds 1mg/mL, the particle size of the nano selenium is almost unchanged. Therefore, the optimal concentration of the sargassum fusiforme polysaccharide modified nano-selenium is determined to be 1mg/mL, and the average particle size of the nano-selenium is 60.9 nm.
In the embodiment, the storage stability of the 1mg/mL sargassum fusiforme polysaccharide-nano selenium and 1mg/mL nano selenium solution is considered, the two solutions are stored in a refrigerator at 4 ℃ for 30 days in a solution form, the obtained nano selenium is observed to be almost completely aggregated and precipitated at the bottom of a bottle, and the supernatant is clarified; the Sargassum fusiforme polysaccharide-nano selenium is still uniformly distributed in the solution, and the solution keeps bright red.
FIG. 3a is a Transmission Electron Microscope (TEM) image of the nano-selenium sol, which shows that nano-selenium without Hizikia fusiforme polysaccharide as diluent is easy to aggregate into stacks, and the particle size is over 100 nm; the Sargassum fusiforme polysaccharide modified nano selenium (shown in figure 3b) has uniform particle size, and the particle size is not more than 100nm when the selenium is uniformly dispersed in the solution.
Fig. 4 is a surface elemental spectrum analysis chart of the sargassum fusiforme functionalized nano-selenium complex, and the result shows that sargassum fusiforme polysaccharide-nano selenium mainly comprises Se element (11.88%), C element (58.57%) and O element (29.55%), which shows that Se element has been successfully incorporated into the polysaccharide matrix. In addition, few distinct absorption peaks of other elements were observed, which demonstrates the purity of hizikia fusiforme polysaccharide nano-selenium.
FIG. 5 shows the UV absorption spectra of Hizikia fusiforme polysaccharide and the functionalized nano-selenium solution of Hizikia fusiforme polysaccharide. Compared with the ultraviolet absorption curve of the sargassum fusiforme polysaccharide solution, the sargassum fusiforme polysaccharide-nano selenium has a lower absorption peak at 200nm, but has a more obvious new absorption peak at 267 nm. The results indicate the formation of SFPS-SeNPs (Sargassum fusiforme polysaccharide functionalized nano-selenium).
EXAMPLE 3 determination of antioxidant Activity of different samples
3.1 Effect of different samples on DPPH radical scavenging
Weighing nano selenium, sargassum fusiforme polysaccharide and sargassum fusiforme polysaccharide functionalized nano selenium powder, respectively dissolving in deionized water to prepare a sample solution (0.1,0.25,0.5,0.75,1,1.5mg/mL) with a certain concentration gradient. And (2) respectively adding 150 mu L of sample solution into 150 mu L of DPPH solution (0.1mM, prepared by absolute ethyl alcohol), uniformly mixing, carrying out light-shielding reaction for 30min at room temperature, measuring the light absorption value at the wavelength of 517nm, using equal volume of distilled water to replace the sample solution as a blank control, and using equal volume of absolute ethyl alcohol to replace the DPPH solution as a sample control. DPPH radical clearance was calculated according to the following formula:
in the formula: a. the0Is the absorbance value of the blank; a. theSIs the absorbance of the sample solution; a. thebAbsorbance of sample control.
FIG. 6a is a bar graph of DPPH clearance for samples of different concentrations, showing that the clearance of DPPH radicals increases with increasing concentration for different samples in the range of 0.1-1.5 mg/ml. Among them, SFPS (hizikia fusiforme polysaccharide) shows the strongest DPPH radical scavenging activity, followed by SFPS-SeNPs (hizikia fusiforme polysaccharide functionalized nano-selenium). The removal rate of SenPs (nano-selenium) has been lower than 30%, showing the lowest DPPH radical scavenging ability.
3.2 scavenging of hydroxyl radicals by different samples
Weighing nano-selenium, sargassum fusiforme polysaccharide and sheepThe powder of the functional nano selenium of the sedum aizoon polysaccharide is dissolved in deionized water to prepare a sample solution (0.1,0.25,0.5,0.75,1,1.5mg/mL) with a certain concentration gradient. Sample solutions with different concentrations, a ferrous sulfate solution with the concentration of 9mM, a salicylic acid solution with the concentration of 9mM prepared by absolute ethyl alcohol and a solution with the concentration of 8.8mM are uniformly mixed according to the volume ratio of 1:1:1:1, and react for 0.5h in a water bath at the temperature of 37 ℃ in a dark place, and then the light absorption value is measured at the position of 510 nm. The blank control was prepared by substituting equal volume of distilled water for the sample solution and H for the same volume of distilled water2O2The solution served as a sample control. Hydroxyl radical clearance was calculated according to the following formula:
in the formula: a. the0Is the absorbance value of the blank; a. theSIs the absorbance of the sample solution; a. thebAbsorbance of sample control.
FIG. 6b is a graph of ABTS clearance of sample solutions of different concentrations, and the results show that the HO-free radical scavenging ability of the sargassum fusiforme polysaccharide and the sargassum fusiforme polysaccharide-nano selenium solution is dose-dependent. The average clearance rate of the sargassum fusiforme polysaccharide reaches 38 percent at 1.5mg/mL, the average clearance rate of the sargassum fusiforme polysaccharide-nano selenium is 30 percent, and the clearance rate of the nano selenium is only 11.5 percent. Sargassum fusiforme polysaccharide still shows the strongest free radical scavenging ability, followed by SFPS-SeNPs, which are the weakest. However, the clearance of hydroxyl radicals by the samples is generally lower compared to the clearance of DPPH.
3.3 scavenging of ABTS free radicals by different samples
Weighing nano selenium, sargassum fusiforme polysaccharide and sargassum fusiforme polysaccharide functionalized nano selenium powder, and dissolving the nano selenium, the sargassum fusiforme polysaccharide and the sargassum fusiforme polysaccharide functionalized nano selenium powder in deionized water to prepare a sample solution (0.1,0.25,0.5,0.75,1,1.5mg/mL) with a certain concentration gradient. Mixing 7mM ABTS solution (2,2' -biazonitrogen-bis-3-ethylbenzthiazoline-6-sulfonic acid) and 2.45mM potassium persulfate in equal volume, and reacting for 16h in a dark place to obtain ABTS working solution. The ABTS working solution was then diluted with PBS buffer (5mM, pH7.4) to give an absorbance of 0.7. + -. 0.02 at 734 nm. Adding 50 μ L sample into 150 μ L LABTS solution, and keeping out lightAfter 6min of reaction, the absorbance at 734nm was measured. Equal volume of distilled water was used to replace the sample solution as a blank control, and equal volume of PBS solution was used to replace H2O2The solution served as a sample control. The ABTS free radical clearance was calculated as follows:
in the formula: a. the0Is the absorbance value of the blank; a. theSIs the absorbance of the sample solution; a. thebAbsorbance of sample control.
FIG. 6c is a result graph of ABTS free radical scavenging rate of samples with different concentrations, and the result shows that the ABTS scavenging capacity of the sargassum fusiforme polysaccharide and the sargassum fusiforme polysaccharide-nano selenium solution is enhanced along with the increase of the concentration, and when the concentration reaches 0.75mg/ml, the scavenging rates of the sargassum fusiforme polysaccharide and the sargassum fusiforme polysaccharide-nano selenium solution reach more than 80%, which shows that the sargassum fusiforme polysaccharide has a strong scavenging effect on ABTS free radicals. Pure SenPs still show poor radical scavenging capacity, with clearance rates of less than 20% at all times.
The result shows that the oxidation resistance of the nano-selenium modified by the sargassum fusiforme polysaccharide is obviously stronger than that of the original nano-selenium, so that the preparation of the nano-selenium by using the sargassum fusiforme polysaccharide as a carrier material is a better choice for improving the stability and the activity of the nano-selenium.
The above examples are only preferred embodiments of the present invention, which are intended to be illustrative and not limiting, and those skilled in the art should understand that they can make various changes, substitutions and alterations without departing from the spirit and scope of the invention.
Claims (10)
1. A preparation method of sargassum fusiforme polysaccharide functionalized nano selenium is characterized by comprising the following steps:
(1) uniformly mixing the sargassum fusiforme polysaccharide solution and the sodium selenite solution, then adding the ascorbic acid solution, uniformly stirring, heating for water bath reaction to obtain a reaction solution;
(2) and (2) dialyzing the reaction solution obtained in the step (1), and freeze-drying to obtain the sargassum fusiforme polysaccharide functionalized nano-selenium.
2. The method for preparing sargassum fusiforme polysaccharide functionalized nano-selenium according to claim 1, wherein the concentration of the sargassum fusiforme polysaccharide solution in the step (1) is 0.25-3 mg/mL.
3. The method for preparing hizikia fusiforme polysaccharide functionalized nano-selenium according to claim 1, wherein the concentration of the sodium selenite solution in the step (1) is 0.01 mol/L.
4. The method for preparing sargassum fusiforme polysaccharide functionalized nano-selenium according to claim 1, wherein the concentration of the ascorbic acid solution in the step (1) is 0.04 mol/L.
5. The method for preparing sargassum fusiforme polysaccharide functionalized nano-selenium according to claim 1, wherein the volume ratio of the sargassum fusiforme polysaccharide solution, the sodium selenite solution and the ascorbic acid solution in the step (1) is 1:1: 1.
6. the method for preparing hizikia fusiforme polysaccharide functionalized nano selenium according to claim 1, wherein the temperature of the water bath reaction in the step (1) is 50 +/-5 ℃, and the time of the water bath reaction is 4 +/-0.5 h.
7. The method for preparing sargassum fusiforme polysaccharide functionalized nano-selenium according to claim 1, wherein the cut-off molecular weight of a dialysis bag adopted in the dialysis treatment in the step (2) is 3-4kD, and the dialysis treatment time is 48-72 h.
8. The method for preparing sargassum fusiforme polysaccharide functionalized nano-selenium according to claim 1, wherein the temperature of the dialysis treatment in the step (2) is 4 ℃.
9. A Sargassum fusiforme polysaccharide functionalized nano-selenium prepared by the preparation method of any one of claims 1-8.
10. The use of the hizikia fusiforme polysaccharide functionalized nano-selenium of claim 9 in the preparation of antioxidant and selenium supplement products.
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