CN113456831B - Method for preparing nano-selenium by using eucommia ulmoides polysaccharide and nano-selenium prepared by method - Google Patents
Method for preparing nano-selenium by using eucommia ulmoides polysaccharide and nano-selenium prepared by method Download PDFInfo
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Abstract
The invention discloses a method for preparing nano-selenium by eucommia ulmoides polysaccharide, which relates to the technical field of nano-materials and comprises the following steps: (1) Preparing eucommia polysaccharide crude extract by taking eucommia leaf or eucommia bark as raw materials; (2) Decolorizing the polysaccharide crude extract with active carbon, purifying with macroporous resin, and drying to obtain eucommia polysaccharide; (3) preparing eucommia polysaccharide nano selenium compound solution; (4) Adding 0.5-1% beta-cyclodextrin into eucommia polysaccharide nanometer selenium compound solution, stirring at room temperature, centrifuging, and freeze drying precipitate to obtain the final product. The invention also provides the nano-selenium prepared by the method. The invention has the beneficial effects that: according to the invention, the nanometer selenium is coated by the eucommia polysaccharide, so that the stability of the eucommia polysaccharide nanometer selenium is improved, and the stability is further enhanced by beta-cyclodextrin loading.
Description
Technical Field
The invention relates to the technical field of nano materials, in particular to a method for preparing nano selenium by eucommia ulmoides polysaccharide and the prepared nano selenium.
Background
Selenium (Se) is one of essential trace elements for human and animals to sustain life, has the effects of resisting oxidation, regulating immunity, promoting animal growth, removing toxic substances, relieving stress and the like, plays a vital role in maintaining body health and regulating diseases, and is known as ' life fire and ' anticancer king '. Selenium entering the human body mainly takes part in the formation of selenoprotein as a structure or active ingredient. These selenoproteins have multiple biological functions, including excellent antioxidant and anti-inflammatory properties, and induction of active thyroid hormones. Because selenoprotein is closely related to various diseases induced by factors such as oxidative stress, inflammation and the like, the selenium content in the human body is maintained to be moderate, and the selenium-rich polypeptide has positive significance in improving the autoimmune power and resisting the oxidative stress and inflammatory diseases. At present, 13 provincial nutrition surveys in China show that the selenium intake of adults is only 26.63 micrograms/day, which is only half of the recommended daily intake. Therefore, the phenomenon of selenium deficiency of people in China at the present stage is common, the selenium supplementing is not slow, and the selenium industry also becomes a new entry point and a new explosion point for detonating the China trillion-level health industry.
The existing forms of selenium in the nature mainly comprise three kinds of inorganic selenium, organic selenium and nano selenium. Compared with inorganic selenium and organic selenium, nano-selenium is the safest and effective selenium supplementing mode due to excellent biological activity, good biocompatibility and lower toxicity, and the synthetic application of nano-selenium is one of the hot spot directions of the current selenium industry research. The preparation method of the nano selenium comprises a physicochemical synthesis method, a microbial reduction method and a plant extract synthesis method. The plant extract is rich in natural polysaccharide, protein and other components, and can be coated on the surface of nano-selenium in the process of reducing inorganic selenium to generate simple substance nano-selenium, so that the double functions of stabilizing nano-selenium and enhancing the biological activity of nano-selenium are achieved. The patent application with publication number of CN109650350A discloses a method for preparing polysaccharide modified nano-selenium on a large scale and application thereof, which discloses that lentinan, chitosan and other polysaccharides are adopted to prepare nano-selenium, and the stability of the nano-selenium modified by the lentinan is good, but the oxidation resistance of the nano-selenium modified by the lentinan is poor.
Disclosure of Invention
The invention aims to solve the technical problems that the nano-selenium modified by lentinan has good stability, but the nano-selenium modified by lentinan has poor oxidation resistance, and provides a preparation method of nano-selenium with uniform particle size, stable structure and good oxidation resistance and the nano-selenium prepared by the preparation method.
The invention solves the technical problems by the following technical means:
a method for preparing nano-selenium by using eucommia ulmoides polysaccharide comprises the following steps:
(1) Preparing eucommia polysaccharide crude extract by taking eucommia leaf or eucommia bark as raw materials;
(2) Decolorizing the polysaccharide crude extract with active carbon, purifying with macroporous resin, and drying to obtain eucommia polysaccharide;
(3) Preparing eucommia polysaccharide solution with mass concentration of 1-2 per mill, adding sodium selenite with mass concentration of 0.1-0.2% and vitamin C with mass concentration of 0.8-1.6%, stirring, standing the reaction mixture in water bath at 40-50deg.C for 4-8 hr, centrifuging, and dissolving the precipitate with deionized water to obtain eucommia polysaccharide nanometer selenium compound solution;
(4) Adding 0.5-1% beta-cyclodextrin into the eucommia polysaccharide nano-selenium compound solution in the step (3), stirring at room temperature, centrifuging, and freeze-drying the precipitate to obtain the product.
The beneficial effects are that: the nano-selenium coated by the eucommia polysaccharide is prepared by the method, the stability of the nano-selenium coated by the eucommia polysaccharide is improved, and the stability is further enhanced by beta-cyclodextrin loading, so that the prepared nano-selenium has uniform particle size and stable structure, the nano-selenium coated by the eucommia polysaccharide has stronger biological activity, and the biological activity of the nano-selenium coated by the eucommia polysaccharide is obviously superior to that of the nano-selenium and the eucommia polysaccharide, and is superior to that of the nano-selenium prepared by lentinan. The nano-selenium provided by the invention has double effects of eucommia polysaccharide and nano-selenium, and has good effects of inhibiting bacteria, diminishing inflammation, resisting oxidation, improving immunity and the like.
The invention synthesizes nano-selenium by adopting the eucommia ulmoides polysaccharide which is an extract of rare medicinal plant eucommia ulmoides in China, and solves the problems that the traditional physicochemical method for synthesizing nano-selenium has high cost, is easy to agglomerate, and the residual chemical medicine in the synthesis process can cause pollution and potential safety hazard.
Preferably, the centrifugal speed in the step (3) and the centrifugal speed in the step (4) are 10000rpm-15000rpm, and the centrifugal time is 10-20min.
Preferably, the preparation method of the eucommia ulmoides polysaccharide crude extract comprises the following steps of: drying folium Eucommiae or cortex Eucommiae, pulverizing, adding into flash extractor at a feed-liquid ratio of 1:15-40, setting voltage of 100-220V, extracting for 1-3 times for 30-60 seconds, mixing filtrates, concentrating under reduced pressure, centrifuging, collecting supernatant, adding absolute ethanol with final ethanol concentration of 75-80%, standing at 4deg.C overnight, and centrifuging to obtain precipitate.
Preferably, the decolorizing with activated carbon comprises the steps of: dissolving eucommia polysaccharide crude extract in phosphoric acid buffer solution, adding active carbon, decolorizing at 50-70deg.C for 1-2 hr, and collecting filtrate to obtain decolorized eucommia polysaccharide crude extract.
Preferably, the eucommia ulmoides polysaccharide crude extract is dissolved in a phosphate buffer solution, the mass concentration of the eucommia ulmoides polysaccharide crude extract is adjusted to be 1-3g/L, and then activated carbon accounting for 0.4-0.8% of the mass of the eucommia ulmoides polysaccharide crude extract is added.
Preferably, the decolorized eucommia polysaccharide crude extract is loaded on macroporous resin, then eluted by 60% -75% ethanol solution, and the filtrate is collected, frozen and dried to obtain eucommia polysaccharide.
The beneficial effects are that: compared with the eucommia ulmoides polysaccharide crude extract and the decolored eucommia ulmoides polysaccharide crude extract, the same amount of sodium selenite is added, and the more the eucommia ulmoides polysaccharide crude extract is subjected to active carbon decoloration and macroporous resin purification, the more the eucommia ulmoides polysaccharide nano-selenium is synthesized.
The invention extracts eucommia ulmoides plant polysaccharide through a flash extractor, and then prepares high-purity eucommia ulmoides polysaccharide through active carbon decolorization and macroporous resin adsorption purification.
Preferably, the loading speed in the step (3) is 1-2mL/min, and the eluting speed is 1-2mL/min.
Preferably, the macroporous resin is one of D-101, DM-130, AB-8, NKA-9, HPD 600.
Preferably, the obtained eucommia polysaccharide is dissolved in 1L of deionized water to prepare eucommia plant polysaccharide solution with mass concentration of 1-2 permillage of polysaccharide, and then 1-2g of sodium selenite and 8-16g of vitamin C are sequentially added.
The invention also provides the nano-selenium prepared by the method.
The invention has the advantages that: the nanometer selenium coated by the eucommia polysaccharide is synthesized, the stability of the nanometer selenium of the eucommia polysaccharide is improved, and the stability is further enhanced by beta-cyclodextrin loading, and the biological activity of the nanometer selenium of the eucommia polysaccharide synthesized by the invention is stronger, and the biological activity of the nanometer selenium coated by the eucommia polysaccharide is obviously better than that of the nanometer selenium and the eucommia polysaccharide and is better than that of the nanometer selenium prepared by lentinan. The nano-selenium provided by the invention has double effects of eucommia polysaccharide and nano-selenium, and has good effects of inhibiting bacteria, diminishing inflammation, resisting oxidation, improving immunity and the like.
The invention synthesizes nano-selenium by adopting the eucommia ulmoides polysaccharide which is an extract of rare medicinal plant eucommia ulmoides in China, and solves the problems that the traditional physicochemical method for synthesizing nano-selenium has high cost, is easy to agglomerate, and the residual chemical medicine in the synthesis process can cause pollution and potential safety hazard.
Compared with the eucommia ulmoides polysaccharide crude extract and the decolored eucommia ulmoides polysaccharide crude extract, the same amount of sodium selenite is added, and the more the eucommia ulmoides polysaccharide crude extract is subjected to active carbon decoloration and macroporous resin purification, the more the eucommia ulmoides polysaccharide nano-selenium is synthesized.
Drawings
Fig. 1 is a scanning electron microscope image of eucommia ulmoides polysaccharide nano-selenium in example 1 of the present invention.
FIG. 2 shows the particle size distribution of eucommia ulmoides polysaccharide nano-selenium in example 1 of the present invention.
Fig. 3 is an EDX spectrum analysis result of nano selenium of eucommia ulmoides polysaccharide in example 1 of the present invention.
FIG. 4 is a graph showing the comparison of the antioxidant capacity of eucommia ulmoides polysaccharide nano-selenium and eucommia ulmoides polysaccharide and chemically synthesized nano-selenium in example 1 of the present invention.
Fig. 5 is a graph showing the comparison of antioxidant properties of nano-selenium synthesized in different ways according to the present invention.
FIG. 6 is a graph showing the comparison of the stability of nanoselenium synthesized in various ways according to the present invention. In the figure, A is comparative example 1, B is comparative example 2, and C is example 1.
FIG. 7 is a graph showing the comparison of the performance of the synthesized nano-selenium before and after purification of eucommia ulmoides polysaccharide of the present invention. In the figure, A is comparative example 3, B is comparative example 4, and C is comparative example 5.
FIG. 8 is a graph showing the results of measuring the purification effect of the activated carbon treatment of different addition amounts on the crude extract of eucommia ulmoides polysaccharide.
Detailed Description
For the purpose of making the objects, technical solutions and advantages of the embodiments of the present invention more apparent, the technical solutions in the embodiments of the present invention will be clearly and completely described in the following in conjunction with the embodiments of the present invention, and it is apparent that the described embodiments are some embodiments of the present invention, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
The test materials, reagents and the like used in the examples described below are commercially available unless otherwise specified.
Those of skill in the art, without any particular mention of the techniques or conditions, may follow the techniques or conditions described in the literature in this field or follow the product specifications.
Example 1
The method for preparing nano-selenium by using eucommia polysaccharide specifically comprises the following steps:
1) The preparation method of the eucommia ulmoides plant polysaccharide crude extract comprises the following steps: drying picked eucommia ulmoides leaves at 50 ℃ for 36 hours, crushing, and sieving with a 60-mesh sieve for standby. Taking a certain amount of water, and adding the water into the flash extractor according to the proportion of the feed liquid ratio of 1:15. The extraction time was set to 30 seconds, the voltage was 100V, and the number of extraction was 1. After the extraction is finished, the filtrates are combined and concentrated under reduced pressure. Subsequently, the mixture was centrifuged at 4000rpm for 5 minutes, and the supernatant was collected. Absolute ethyl alcohol is added into the supernatant fluid to ensure that the final concentration of the ethyl alcohol is 75 percent, the mixture is stood at 4 ℃ overnight and centrifuged at 10000rpm for 10 minutes, and the obtained precipitate is the eucommia polysaccharide crude extract.
2) Decolorizing cortex Eucommiae plant polysaccharide crude extract with active carbon: the eucommia polysaccharide crude extract prepared in 1) was dissolved in a phosphate buffer solution (pH 5.0) so that the polysaccharide mass concentration was 1g/L. Adding active carbon with the mass of 0.4% of that of the crude polysaccharide, decolorizing at 50deg.C for 1 hr, vacuum filtering, and collecting filtrate to obtain decolorized crude extract of eucommia ulmoides plant polysaccharide.
3) Purifying the eucommia ulmoides plant polysaccharide crude extract: 2) The crude eucommia ulmoides plant polysaccharide extract prepared in the method is loaded into macroporous resin (D-101) at a speed of 1.0 mL/min, 60% ethanol solution is adopted, elution is carried out at a flow speed of 1.0 mL/min, filtrate is collected, and freeze drying is carried out, so that purified eucommia ulmoides plant polysaccharide freeze-dried powder is obtained, and the polysaccharide yield is calculated.
4) The synthesis of eucommia polysaccharide nano selenium compound: dissolving the eucommia ulmoides plant polysaccharide freeze-dried powder prepared in the step 3) in 1L of deionized water to prepare eucommia ulmoides plant polysaccharide solution with mass concentration of 1%o. Then, sequentially adding 1g of sodium selenite and 8g of vitamin C (Vc), stirring uniformly, placing the reaction mixture in a water bath at 40 ℃ for standing reaction for 4 hours, centrifuging at 10000rpm for 10 minutes, and dissolving the obtained precipitate with deionized water to obtain the eucommia polysaccharide nano-selenium compound solution.
5) Further functionalization of eucommia ulmoides polysaccharide nano-selenium compound: adding 0.5 per mill of beta-cyclodextrin into the eucommia polysaccharide nano-selenium compound solution obtained in the step 4), stirring for 2 hours at room temperature, centrifuging at 10000rpm for 10 minutes, and freeze-drying the obtained precipitate to obtain the eucommia polysaccharide nano-selenium compound functionalized by the beta-cyclodextrin.
Experimental results: with the conditions in this example, the yield of eucommia polysaccharide was 1.94%.
Example 2
The method for preparing nano-selenium by using eucommia polysaccharide specifically comprises the following steps:
1) The preparation method of the eucommia ulmoides plant polysaccharide crude extract comprises the following steps: drying picked eucommia ulmoides leaves at 60 ℃ for 40 hours, crushing, and sieving with a 60-mesh sieve for standby. Taking a certain amount of water, and adding the water into the flash extractor according to the proportion of the feed liquid ratio of 1:30. The extraction time was set at 40 seconds, the voltage at 160V, and the number of extractions was 2. After the extraction is finished, the filtrates are combined and concentrated under reduced pressure. Subsequently, the mixture was centrifuged at 4500rpm for 10 minutes, and the supernatant was collected. Absolute ethyl alcohol is added into the supernatant fluid to lead the final concentration of the ethyl alcohol to be 75 percent, the mixture is stood at 4 ℃ overnight and centrifuged at 15000rpm for 20 minutes, and the obtained precipitate is the eucommia polysaccharide crude extract.
2) Decolorizing cortex Eucommiae plant polysaccharide crude extract with active carbon: the eucommia polysaccharide crude extract prepared in 1) was dissolved in a phosphate buffer solution (pH 5.0) so that the mass concentration of polysaccharide was 2g/L. Adding active carbon with the mass of 0.5% of that of the crude polysaccharide, decolorizing at 60 ℃ for 2 hours, filtering, and collecting filtrate to obtain the decolorized crude extract of eucommia ulmoides plant polysaccharide.
3) Purifying the eucommia ulmoides plant polysaccharide crude extract: 2) The crude eucommia ulmoides plant polysaccharide extract prepared in the method is loaded into macroporous resin (AB-8) at a speed of 1.0 mL/min, a 75% ethanol solution is adopted, elution is carried out at a flow speed of 1.0 mL/min, a filtrate is collected, and freeze drying is carried out, so that purified eucommia ulmoides plant polysaccharide freeze-dried powder is obtained, and the polysaccharide yield is calculated.
4) The synthesis of eucommia polysaccharide nano selenium compound: dissolving the eucommia ulmoides plant polysaccharide freeze-dried powder prepared in the step 3) in 1L of deionized water to prepare eucommia ulmoides plant polysaccharide solution with the mass concentration of 1.5 per mill. Then, sequentially adding 1.5g of sodium selenite and 12g of vitamin C (Vc), stirring uniformly, placing the reaction mixture in a water bath at 45 ℃ for standing reaction for 8 hours, centrifuging at 15000rpm for 20 minutes, and dissolving the obtained precipitate with deionized water to obtain the eucommia polysaccharide nano-selenium compound solution.
5) Further functionalization of eucommia ulmoides polysaccharide nano-selenium compound: adding 0.8%o beta-cyclodextrin into the eucommia polysaccharide nano selenium compound solution obtained in the step 4), stirring for 4 hours at room temperature, centrifuging at 15000rpm for 20 minutes, and freeze-drying the obtained precipitate to obtain the eucommia polysaccharide nano selenium compound functionalized by the beta-cyclodextrin.
Experimental results: with the conditions in this example, the yield of eucommia polysaccharide was 3.26%.
Example 3
The method for preparing nano-selenium by using eucommia polysaccharide specifically comprises the following steps:
1) The preparation method of the eucommia ulmoides plant polysaccharide crude extract comprises the following steps: drying picked eucommia ulmoides leaves at 70 ℃ for 48 hours, crushing, and sieving with a 60-mesh sieve for standby. Taking a certain amount of water, and adding the water into the flash extractor according to the ratio of the feed liquid to the liquid of 1:40. The extraction time was set to 60 seconds, the voltage 220V, and the number of extraction times was 3. After the extraction is finished, the filtrates are combined and concentrated under reduced pressure. Subsequently, the mixture was centrifuged at 5000rpm for 5 minutes, and the supernatant was collected. Absolute ethyl alcohol is added into the supernatant fluid to ensure that the final concentration of the ethyl alcohol is 80 percent, the mixture is stood overnight at 4 ℃ and centrifuged at 15000rpm for 10 minutes, and the obtained precipitate is the eucommia polysaccharide crude extract.
2) Decolorizing cortex Eucommiae plant polysaccharide crude extract with active carbon: the eucommia polysaccharide crude extract prepared in 1) was dissolved in a phosphate buffer solution (pH 5.0) so that the polysaccharide mass concentration was 3g/L. Adding active carbon equivalent to 0.8% of crude polysaccharide, decolorizing at 70deg.C for 1 hr, vacuum filtering, and collecting filtrate to obtain decolorized crude extract of eucommia ulmoides plant polysaccharide.
3) Purifying the eucommia ulmoides plant polysaccharide crude extract: 2) The crude extract of eucommia ulmoides plant polysaccharide prepared in the method is loaded into macroporous resin NKA-9 at a speed of 1.0-2.0 mL/min, 60% ethanol solution is adopted, elution is carried out at a flow speed of 1.5mL min, filtrate is collected, freeze-drying is carried out, and purified eucommia ulmoides plant polysaccharide freeze-dried powder is obtained, and polysaccharide yield is calculated.
4) The synthesis of eucommia polysaccharide nano selenium compound: dissolving the eucommia ulmoides plant polysaccharide freeze-dried powder prepared in the step 3) in 1L of deionized water to prepare eucommia ulmoides plant polysaccharide solution with the mass concentration of 0.1%. Then, sequentially adding 2g of sodium selenite and 16g of vitamin C (Vc), uniformly stirring, standing the reaction mixture in a water bath at 50 ℃ for 6 hours, centrifuging at 10000rpm for 20 minutes, and dissolving the obtained precipitate with deionized water to obtain the eucommia polysaccharide nano-selenium compound solution.
5) Further functionalization of eucommia ulmoides polysaccharide nano-selenium compound: adding 1%o beta-cyclodextrin into the eucommia polysaccharide nano selenium compound solution obtained in the step 4), stirring for 4 hours at room temperature, centrifuging at 15000rpm for 20 minutes, and freeze-drying the obtained precipitate to obtain the eucommia polysaccharide nano selenium compound functionalized by the beta-cyclodextrin.
Experimental results: with the conditions in this example, the yield of eucommia polysaccharide was 2.21%.
Example 4
This embodiment differs from embodiment 1 in that: the eucommia ulmoides leaves are replaced by eucommia ulmoides bark.
Example 5
This embodiment differs from embodiment 1 in that: the addition amount of the activated carbon was adjusted to 0.6%.
Comparative example 1
The nano selenium is synthesized by adopting a chemical synthesis method. Cysteine with the concentration of 25mM is dropwise added to 10mL of 1M Na under the action of a magnetic stirrer 2 And (3) in the SeO solution, distilled water is used for constant volume to 25ml, the reaction is carried out for 30min at room temperature, and the centrifugation is carried out for 20min at 10000rpm, so that the obtained red precipitate is the nano-selenium prepared by a chemical method.
Comparative example 2
This comparative example differs from example 1 in that: and (3) freeze-drying the eucommia ulmoides polysaccharide nano-selenium compound solution in the step (4).
Comparative example 3
1) The preparation method of the eucommia ulmoides plant polysaccharide crude extract comprises the following steps: drying picked eucommia ulmoides leaves at 50 ℃ for 36 hours, crushing, and sieving with a 60-mesh sieve for standby. Taking a certain amount of water, and adding the water into the flash extractor according to the proportion of the feed liquid ratio of 1:15. The extraction time was set to 30 seconds, the voltage was 100V, and the number of extraction was 1. After the extraction is finished, the filtrates are combined and concentrated under reduced pressure. Subsequently, the mixture was centrifuged at 4000rpm for 5 minutes, and the supernatant was collected. Absolute ethyl alcohol is added into the supernatant fluid to ensure that the final concentration of the ethyl alcohol is 75 percent, the mixture is stood at 4 ℃ overnight and centrifuged at 10000rpm for 10 minutes, and the obtained precipitate is the eucommia polysaccharide crude extract.
2) The synthesis of eucommia polysaccharide nano selenium compound: dissolving the eucommia ulmoides polysaccharide crude extract prepared in the step 1) in 1L of deionized water to prepare eucommia ulmoides plant polysaccharide solution with mass concentration of 1%o. Then, sequentially adding 1g of sodium selenite and 8g of vitamin C (Vc), stirring uniformly, placing the reaction mixture in a water bath at 40 ℃ for standing reaction for 4 hours, centrifuging at 10000rpm for 10 minutes, and dissolving the obtained precipitate with deionized water to obtain the eucommia polysaccharide nano-selenium compound solution.
3) Further functionalization of eucommia ulmoides polysaccharide nano-selenium compound: adding 0.5 per mill of beta-cyclodextrin into the eucommia polysaccharide nano-selenium compound solution obtained in the step 2), stirring for 2 hours at room temperature, centrifuging at 10000rpm for 10 minutes, and freeze-drying the obtained precipitate to obtain the eucommia polysaccharide nano-selenium compound functionalized by the beta-cyclodextrin.
Comparative example 4
1) The preparation method of the eucommia ulmoides plant polysaccharide crude extract comprises the following steps: drying picked eucommia ulmoides leaves at 50 ℃ for 36 hours, crushing, and sieving with a 60-mesh sieve for standby. Taking a certain amount of water, and adding the water into the flash extractor according to the proportion of the feed liquid ratio of 1:15. The extraction time was set to 30 seconds, the voltage was 100V, and the number of extraction was 1. After the extraction is finished, the filtrates are combined and concentrated under reduced pressure. Subsequently, the mixture was centrifuged at 4000rpm for 5 minutes, and the supernatant was collected. Absolute ethyl alcohol is added into the supernatant fluid to ensure that the final concentration of the ethyl alcohol is 75 percent, the mixture is stood at 4 ℃ overnight and centrifuged at 10000rpm for 10 minutes, and the obtained precipitate is the eucommia polysaccharide crude extract.
2) Decolorizing cortex Eucommiae plant polysaccharide crude extract with active carbon: 1) The crude eucommia polysaccharide extract prepared in the method is dissolved in a phosphoric acid buffer solution (pH 5.0) so that the mass concentration of polysaccharide is 1g/L. Adding active carbon with the mass of 0.4% of that of the crude polysaccharide, decolorizing at 50deg.C for 1 hr, vacuum filtering, collecting filtrate, and freeze drying to obtain decolorized crude extract of eucommia ulmoides plant polysaccharide.
3) The synthesis of eucommia polysaccharide nano selenium compound: dissolving the eucommia ulmoides plant polysaccharide crude extract prepared in the step 2) in 1L of deionized water to prepare eucommia ulmoides plant polysaccharide solution with mass concentration of 1%o. Then, sequentially adding 1g of sodium selenite and 8g of vitamin C (Vc), stirring uniformly, placing the reaction mixture in a water bath at 40 ℃ for standing reaction for 4 hours, centrifuging at 10000rpm for 10 minutes, and dissolving the obtained precipitate with deionized water to obtain the eucommia polysaccharide nano-selenium compound solution.
4) Further functionalization of eucommia ulmoides polysaccharide nano-selenium compound: adding 0.5 per mill of beta-cyclodextrin into the eucommia polysaccharide nano-selenium compound solution obtained in the step 3), stirring for 2 hours at room temperature, centrifuging at 10000rpm for 10 minutes, and freeze-drying the obtained precipitate to obtain the eucommia polysaccharide nano-selenium compound functionalized by the beta-cyclodextrin.
Comparative example 5
The comparative example uses chitosan to prepare nano-selenium, and eucommia polysaccharide is replaced by chitosan with the same content (purchased from Beijing Soy Bao technology Co., ltd.) on the basis of example 1.
Comparative example 6
The comparative example uses lentinan to prepare nano-selenium, and the eucommia ulmoides polysaccharide is replaced by lentinan with the same content (purchased from Changsha health biotechnology Co., ltd.) on the basis of example 1.
Comparative example 7
This comparative example differs from example 1 in that: the addition amount of the activated carbon was adjusted to 0.2%.
Comparative example 8
This comparative example differs from example 1 in that: the addition amount of the activated carbon was adjusted to 0.3%.
Experimental data and analysis:
detecting the particle size of the eucommia polysaccharide nano-selenium compound by using a Markov laser particle size tester (DLS). And observing the size and dispersion condition of the eucommia ulmoides polysaccharide nano-selenium compound by adopting a scanning electron microscope. And (3) characterizing the element content in the eucommia polysaccharide nano-selenium sample by using an energy spectrometer (EDS). And (3) adopting a Fourier transform infrared spectrometer (FTIR) to characterize the functional group composition in the eucommia ulmoides polysaccharide nano-selenium sample. Referring to national standard GB/T39100-2020, the antioxidant capacity of eucommia polysaccharide nano-selenium is evaluated by adopting a DPPH free radical scavenging capacity test. The measurement methods of the laser particle sizer, the scanning electron microscope, and the spectrometer are all prior art.
The nanometer selenium of eucommia ulmoides polysaccharide in example 1 is shown in figure 1, and the particle size range is 20-50nm. By adopting a scanning electron microscope and an energy spectrometer (SEM-EDX), as shown in fig. 2 and 3, nano particles with the particle size of 20-50nm are observed, and the EDX energy spectrum shows a characteristic peak of Se, which indicates that the prepared nano particles are nano selenium particles.
The particle size results of the eucommia ulmoides polysaccharide nano-selenium compound detected by a Markov laser particle size tester (DLS) show that the particle size of the eucommia ulmoides polysaccharide nano-selenium compound synthesized in the embodiment 2 is 30-50nm.
The particle size results of the eucommia ulmoides polysaccharide nano-selenium compound detected by a Markov laser particle size tester (DLS) show that the particle size of the eucommia ulmoides polysaccharide nano-selenium compound synthesized in the embodiment 3 is 50-80nm.
As shown in fig. 4, the eucommia polysaccharide nano-selenium DPPH free radical scavenging ability of the eucommia polysaccharide synthesized in example 1 is significantly higher than the pure eucommia polysaccharide scavenging effect of example 1 and higher than the nano-selenium synthesized by the chemical method of comparative example 1 at different concentrations due to the synergistic effect of the eucommia polysaccharide and the nano-selenium. Wherein the abscissa in FIG. 4 represents the concentrations of eucommia polysaccharide, eucommia polysaccharide nano-selenium, and chemically synthesized nano-selenium in comparative example 1.
As shown in FIG. 5, when the concentration of polysaccharide nano-selenium is 1mg/mL, the oxidation resistance of eucommia ulmoides polysaccharide nano-selenium is better than that of chitosan nano-selenium and lentinan nano-selenium.
Figure 6 is a comparison of stability of nanoselenium synthesized in different ways. In the figure, A is comparative example 1, B is comparative example 2, and C is example 1. It can be seen that the nano-selenium water solution has granular sediment at the bottom of A, B after standing for 1 day, which is formed by nano-selenium agglomeration. And C, nano selenium agglomeration does not exist, eucommia polysaccharide nano selenium is uniformly distributed in the solution, and the stability is obviously improved after beta-cyclodextrin is loaded.
FIG. 7 is a comparison of the performance of the synthesized nano-selenium before and after purification of eucommia ulmoides polysaccharide. In the figure, A is comparative example 3, nanometer selenium is synthesized by adopting crude eucommia polysaccharide extract, B is comparative example 4, nanometer selenium is synthesized by adopting crude eucommia polysaccharide extract decolorized by active carbon, C is comparative example 5, eucommia polysaccharide purified by active carbon decolorization and macroporous resin is adopted, the addition amount of the extract in A, B, C is 1g/L, and the addition amount of sodium selenite is 2mM. The darker the color, the more the amount of synthesized eucommia polysaccharide nano-selenium.
FIG. 8 shows the effect of the treatment with activated carbon in different amounts on the purification effect of crude eucommia polysaccharide extract, wherein the polysaccharide content and impurity content of crude eucommia polysaccharide extract without purification treatment were set to 100%. When the addition amount of activated carbon was 0.5%, the polysaccharide yield was higher, but when the addition amount of activated carbon was increased, the polysaccharide yield was decreased.
The above embodiments are only for illustrating the technical solution of the present invention, and are not limiting; although the invention has been described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that: the technical scheme described in the foregoing embodiments can be modified or some technical features thereof can be replaced by equivalents; such modifications and substitutions do not depart from the spirit and scope of the technical solutions of the embodiments of the present invention.
Claims (10)
1. A method for preparing nano-selenium by using eucommia ulmoides polysaccharide is characterized by comprising the following steps: the method comprises the following steps:
(1) Preparing eucommia polysaccharide crude extract by taking eucommia leaf or eucommia bark as raw materials;
(2) Decolorizing the polysaccharide crude extract with active carbon, purifying with macroporous resin, and drying to obtain eucommia polysaccharide;
(3) Preparing eucommia polysaccharide solution with mass concentration of 1-2 per mill, adding sodium selenite with mass concentration of 0.1-0.2% and vitamin C with mass concentration of 0.8-1.6%, stirring, standing the reaction mixture in water bath at 40-50deg.C for 4-8 hr, centrifuging, and dissolving the precipitate with deionized water to obtain eucommia polysaccharide nanometer selenium compound solution;
(4) Adding 0.5-1% beta-cyclodextrin into the eucommia polysaccharide nano-selenium compound solution in the step (3), stirring at room temperature, centrifuging, and freeze-drying the precipitate to obtain the product.
2. The method for preparing nano-selenium by using eucommia polysaccharide according to claim 1, wherein the method comprises the following steps: the centrifugal rotational speeds in the step (3) and the step (4) are 10000rpm-15000rpm, and the centrifugal time is 10-20min.
3. The method for preparing nano-selenium by using eucommia polysaccharide according to claim 1, wherein the method comprises the following steps: the preparation method of the eucommia ulmoides polysaccharide crude extract comprises the following steps: drying folium Eucommiae or cortex Eucommiae, pulverizing, adding into flash extractor at a feed-liquid ratio of 1:15-40, setting voltage of 100-220V, extracting for 1-3 times for 30-60 seconds, mixing filtrates, concentrating under reduced pressure, centrifuging, collecting supernatant, adding absolute ethanol with final ethanol concentration of 75-80%, standing at 4deg.C overnight, and centrifuging to obtain precipitate.
4. The method for preparing nano-selenium by using eucommia polysaccharide according to claim 1, wherein the method comprises the following steps: the active carbon is adopted for decoloring, which comprises the following steps: dissolving eucommia polysaccharide crude extract in phosphoric acid buffer solution, adding active carbon, decolorizing at 50-70deg.C for 1-2 hr, and collecting filtrate to obtain decolorized eucommia polysaccharide crude extract.
5. The method for preparing nano-selenium by using eucommia polysaccharide according to claim 4, wherein the method comprises the following steps: dissolving eucommia ulmoides polysaccharide crude extract in phosphoric acid buffer solution, adjusting the mass concentration of the polysaccharide crude extract to 1-3g/L, and then adding activated carbon accounting for 0.4-0.8% of the mass of the eucommia ulmoides polysaccharide crude extract.
6. The method for preparing nano-selenium by using eucommia polysaccharide according to claim 1, wherein the method comprises the following steps: loading the decolorized crude extract of eucommia ulmoides polysaccharide onto macroporous resin, eluting with 60% -75% ethanol solution, collecting filtrate, and lyophilizing to obtain eucommia ulmoides polysaccharide.
7. The method for preparing nano-selenium by using eucommia polysaccharide according to claim 6, wherein the method comprises the following steps: the loading speed in the step (3) is 1-2mL/min, and the eluting speed is 1-2mL/min.
8. The method for preparing nano-selenium by using eucommia polysaccharide according to claim 6, wherein the method comprises the following steps: the macroporous resin is one of D-101, DM-130, AB-8, NKA-9 and HPD 600.
9. The method for preparing nano-selenium by using eucommia polysaccharide according to claim 1, wherein the method comprises the following steps: dissolving the obtained eucommia ulmoides polysaccharide in 1L deionized water to prepare eucommia ulmoides plant polysaccharide solution with mass concentration of 1-2 permillage polysaccharide, and sequentially adding 1-2g sodium selenite and 8-16g vitamin C.
10. Nano-selenium obtainable by the process of any of claims 1-9.
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