Tea polyphenol nano-selenium particles as well as preparation method and application thereof
Tea polyphenol nanoselenium particles prepared through tea polyphenol modification and reduction reaction solve the problems of instability of inorganic selenium nanoparticles and low bioavailability of tea polyphenols, achieve the improvement of stability and bioavailability, and have good antioxidant properties and aluminum ion adsorption ability.
Patent Information
- Application Number
- CN202510085809.7
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2025-01-20
- Publication Date
- 2025-04-25
AI Technical Summary
The existing inorganic selenium nanoparticles are unstable and are prone to aggregate into gray or black monomer selenium, with low biological activity. At the same time, tea polyphenols are easily oxidized, alkaline conditions are unstable, and the metabolic rate in the biological system is high, resulting in low bioavailability.
The surface modification of the selenium nanoparticles was prepared by introducing tea polyphenols, and the reduction reaction was used to convert SeO32- into nanoSe to prepare stable tea polyphenol nanoselenium particles.
The stability of selenium nanoparticles has been improved, the problems of oxidation and low bioavailability of tea polyphenols are avoided, the antioxidant performance, bioavailability and biocompatibility of tea polyphenol nanoselenium particles are enhanced, and the ability to adsorb or remove aluminum ions is excellent.
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Abstract
Description
Technical Field
[0001] The invention belongs to the technical field of nanoparticles, and specifically relates to tea polyphenol nano-selenium particles and a preparation method and application thereof. Background Art
[0002] As a micronutrient necessary for maintaining normal physiological functions of the human body, selenium is closely related to the occurrence and development of cardiovascular diseases, chronic metabolic diseases, liver fibrosis, arthritis, and cancer. It has anti-inflammatory, antioxidant, and immunomodulatory properties. However, selenium is a double-edged sword because the threshold between beneficial and toxic doses is narrow, and overdose may lead to toxicity. In addition, the form of selenium also affects its toxicity and bioactivity. At present, selenium mainly includes inorganic selenium, organic selenium, and nano-selenium. The low bioavailability and high toxicity of inorganic selenium limit its application and promotion in medicine and food. The subchronic toxic dose of organic selenium is comparable to that of inorganic selenium, but its manufacturing process is complex, the production cost is high, and its actual application is less. In contrast, selenium nanoparticles (SeNPs) formed by nano-formation have better antioxidant properties, lower toxicity, higher bioavailability, and biocompatibility, and have recently gained widespread interest and application in the biomedical field.
[0003] However, zero-valent red SeNPs converted from inorganic selenium are unstable and easily aggregate into gray or black monomeric selenium, which is more stable, almost insoluble in water, and has low biological activity. Summary of the invention
[0004] The present invention provides a tea polyphenol nano-selenium particle and a preparation method and application thereof, which effectively solves the defect of instability of zero-valent red selenium nanoparticles converted from inorganic selenium in the prior art, and uses tea polyphenol as a modifier, thereby avoiding the technical problems of tea polyphenol being easily oxidized, unstable under alkaline conditions, and having a high metabolic rate in the biological system, which leads to low bioavailability of tea polyphenol. In the present invention, by introducing tea polyphenol to modify the surface of SeNPs, it has been found that a stable surface-covered or nested dispersant-nanoselenium form can be produced by entering the reaction system.
[0005] The first object of the present invention is to provide a method for preparing tea polyphenol nano-selenium particles, comprising the following steps: 2- The source is used as the raw material for the reduction reaction, and SeO3 2- Converted into nano-Se to obtain tea polyphenol nano-selenium particles.
[0006] As a preferred embodiment, SeO3 is added to the tea polyphenol solution 2- The substance is subjected to reduction reaction at 45°C to 55°C for 3 to 5 hours to obtain tea polyphenol nano-selenium particles.
[0007] As a preferred embodiment, the SeO32- The substance is sodium selenite, the concentration of the tea polyphenol solution is 2.5-3.0 g / L, and the mass ratio of the sodium selenite to the tea polyphenol solution is 1:0.22-0.34.
[0008] In order to obtain a higher yield of nano-selenium, the reduction reaction time is controlled to 3 to 5 hours. If the heating time exceeds 5 hours or is less than 3 hours, the yield of tea polyphenols selenium nanoparticles will be affected. If the heating time is less than 3 hours, the reaction is not complete, reflecting that the prepared tea polyphenols selenium nanoparticles are relatively small; if the heating time exceeds 5 hours, the prepared nano-selenium will be further reduced, resulting in a lower yield of the prepared tea polyphenols selenium nanoparticles.
[0009] As a preferred embodiment, the tea polyphenol solution is specifically prepared by mixing green tea powder with a methanol solution having a volume fraction of 65% to 75%, extracting at 65° C. to 75° C. for 8 to 12 minutes, collecting the extract, and filtering to obtain the tea polyphenol solution.
[0010] As a preferred embodiment, the mass volume ratio of the green tea powder and the methanol solution is 1g:40mL-60mL.
[0011] As a preferred embodiment, the extraction is performed 1 to 3 times.
[0012] As a preferred embodiment, the particle size of the tea polyphenol nano-selenium is 205.573nm to 227.027nm.
[0013] The second object of the present invention is to provide tea polyphenol nano-selenium particles prepared by the above preparation method.
[0014] The third object of the present invention is to provide an application of the tea polyphenol nano-selenium particles in removing aluminum ions from wastewater.
[0015] Compared with the prior art, the present invention has the following beneficial effects:
[0016] The present invention introduces tea polyphenols to modify the surface of selenium nanoparticles (SeNPs), thereby obtaining a stable surface-covered or nested dispersant-nanoselenium form, and the prepared tea polyphenols selenium nanoparticles have better antioxidant properties, lower toxicity, higher bioavailability and biocompatibility. The preparation method of tea polyphenols selenium nanoparticles provided by the present invention not only prevents zero-valent red elemental selenium from easily aggregating into gray or black monomeric selenium, but also solves the technical problem that tea polyphenols are easily oxidized, and shows a significant effect in improving the stability of tea polyphenols and elemental selenium and enhancing the expression of biological activity.
[0017] The tea polyphenol nano-selenium particles prepared in the present invention also have excellent ability to adsorb or remove aluminum ions. BRIEF DESCRIPTION OF THE DRAWINGS
[0018] Figure 1 This is a flow chart for preparing tea polyphenol selenium nanoparticles according to Example 1 of the present invention.
[0019] Figure 2 The results are bar graphs showing the particle size, potential, selenium conversion rate, and total antioxidant capacity of tea polyphenol nano-selenium under different sodium selenite concentrations. Figure 2 Figure A in the figure shows a bar chart of the particle size of tea polyphenol nano-selenium measured at different sodium selenite concentrations; Figure 2 Figure B in the figure is a bar graph showing the results of measuring the potential of tea polyphenol nano-selenium at different concentrations of sodium selenite; Figure 2 Figure C in the figure is a bar chart showing the results of measuring the selenium conversion rate of tea polyphenol nano-selenium at different sodium selenite concentrations; Figure 2 Figure D is a bar graph showing the results of measuring the total antioxidant capacity of tea polyphenol nano-selenium at different concentrations of sodium selenite.
[0020] Figure 3 The results of the effects of different temperatures on the particle size and potential of tea polyphenol nano-selenium; Figure 3 Figure A in the figure shows a bar chart of the particle size determination results of tea polyphenol nano-selenium at different temperatures; Figure 3 Figure B is a bar graph showing the measurement results of the potential of tea polyphenol nano-selenium at different temperatures.
[0021] Figure 4 The figure shows the effect of different pH values on the particle size and potential of tea polyphenol nano-selenium. Figure 4 Figure A in the figure shows a bar chart of the particle size determination results of tea polyphenol nano-selenium at different pH values; Figure 4 Figure B is a bar graph showing the measurement results of the potential of tea polyphenol nano-selenium at different pH values.
[0022] Figure 5 It is a bar chart of the storage stability test results of tea polyphenols nano-selenium; Figure 5 Figure A in the figure shows a bar chart showing the results of measuring the particle size of tea polyphenol nano-selenium during storage for 48 days; Figure 5 Figure B is a bar graph showing the results of measuring the nano-selenium potential of tea polyphenols during storage for 48 days.
[0023] Figure 6 for Na + The results of the effect on the tea polyphenol nano-selenium stabilization system; Figure 6 Figure A shows that in Na + The bar graph of the particle size determination results of tea polyphenols nano-selenium under the influence of Figure 6 Figure B shows that in Na +Bar graph of the measurement results of the potential of tea polyphenol nano-selenium under the influence of.
[0024] Figure 7 K + The results of the effect on the tea polyphenol nano-selenium stabilization system; Figure 7 The A in K + The bar graph of the particle size determination results of tea polyphenols nano-selenium under the influence of Figure 7 The B in K + Bar graph of the measurement results of the potential of tea polyphenol nano-selenium under the influence of.
[0025] Figure 8 Mg 2+ The results of the effect on the tea polyphenol nano-selenium stabilization system; Figure 8 Figure A shows that in Mg 2+ The bar graph of the particle size determination results of tea polyphenols nano-selenium under the influence of Figure 8 Figure B shows that in Mg 2+ Bar graph of the measurement results of the potential of tea polyphenol nano-selenium under the influence of.
[0026] Fig. 9 Mg 2+ The results of the effect on the tea polyphenol nano-selenium stabilization system; Fig. 9 Figure A shows that in Mg 2+ The bar graph of the particle size determination results of tea polyphenols nano-selenium under the influence of Fig. 9 Figure B shows that in Mg 2+ Bar graph of the measurement results of the potential of tea polyphenol nano-selenium under the influence of.
[0027] Fig.10 Zn 2+ The results of the effect on the tea polyphenol nano-selenium stabilization system; Fig.10 Figure A shows that in Zn 2+ The bar graph of the particle size determination results of tea polyphenols nano-selenium under the influence of Fig.10 Figure B shows that in Zn 2+ Bar graph of the measurement results of the potential of tea polyphenol nano-selenium under the influence of.
[0028] Fig.11 Fe 2+ The results of the effect on the tea polyphenol nano-selenium stabilization system; Fig.11 Figure A shows that in Fe 2+ The bar graph of the particle size determination results of tea polyphenols nano-selenium under the influence of Fig.11 Figure B shows that in Fe 2+ Bar graph of the measurement results of the potential of tea polyphenol nano-selenium under the influence of.
[0029] Fig.12This is the analysis result of the ability of tea polyphenol nano-selenium to remove aluminum ions; Fig.12 Figure A shows the effects of different tea polyphenol nano-selenium contents on the removal of Al 3+ Histogram of capability test results; Fig.12 Figure B shows different Al 3+ Concentration, remove Al 3+ Histogram of capability test results. DETAILED DESCRIPTION
[0030] The present invention is described in detail below in conjunction with specific examples, but it should not be construed as limiting the present invention. Unless otherwise specified, the technical means used in the following examples are conventional means well known to those skilled in the art, and the materials, reagents, etc. used in the following examples, unless otherwise specified, can be obtained from commercial sources.
[0031] In view of the problems mentioned in the background technology of the present invention: tea polyphenols are easily oxidized, alkaline conditions are unstable, and the metabolic rate in the biological system is high, resulting in low bioavailability of tea polyphenols, which limits the expansion of tea polyphenols from the laboratory to the practical application field. Based on the above technical problems, the present invention provides a tea polyphenols nano-selenium particle and a preparation method and application thereof.
[0032] The technical contents of the present invention are described in detail below.
[0033] 1. Experimental Materials
[0034] The tea powder used in the present invention is made from green tea of the variety "Chunbo Green".
[0035] Example 1
[0036] A method for preparing tea polyphenol nano-selenium, the preparation process is as follows Figure 1 As shown, the following steps are included:
[0037] Preparation of tea polyphenols: Weigh tea powder and use methanol with a concentration of 100% to extract tea polyphenols through a water bath, remove the supernatant solution, and obtain a tea polyphenol solution. The specific method is as follows:
[0038] S1, crush the green tea "Chunbo Green" into tea powder, pass through an 80-mesh sieve, weigh 1g (accurate to 0.0001g) of tea powder into a 50mL centrifuge tube, add 25mL of 70% methanol aqueous solution preheated at 70℃, stir well with a glass to moisten, immediately transfer to a 70℃ water bath for 10min (stir once every 5min), cool to room temperature after leaching, centrifuge at 3500r / min for 10min, and transfer the supernatant to a 50mL volumetric flask. The residue is extracted once with 25mL of 70% methanol aqueous solution, and the above operation is repeated. Combine the extracts to make up to 50mL, shake well, filter with a 0.45μm membrane, and obtain a tea polyphenol solution for standby use (the extract can be stored at 4℃ for up to 24h).
[0039] S2, preparing tea polyphenol nano-selenium: adding 0.1 g of sodium selenite to 50 mL of the tea polyphenol solution, and incubating the mixture in a water bath at 50° C. for 4 h to obtain tea polyphenol nano-selenium particles.
[0040] Example 2
[0041] A method for preparing tea polyphenol nano-selenium comprises the following steps:
[0042] S1, crush the green tea "Chunbo Green" into tea powder, pass through an 80-mesh sieve, weigh 1g (accurate to 0.0001g) of tea powder into a 50mL centrifuge tube, add 25mL of 70% methanol aqueous solution preheated at 70℃, stir well with a glass to moisten, immediately transfer to a 70℃ water bath for 10min (stir once every 5min), cool to room temperature after leaching, centrifuge at 3500r / min for 10min, and transfer the supernatant to a 50mL volumetric flask. The residue is extracted once with 25mL of 70% methanol aqueous solution, and the above operation is repeated. Combine the extracts to make up to 50mL, shake well, filter with a 0.45μm membrane, and obtain a tea polyphenol solution for standby use (the extract can be stored at 4℃ for up to 24h).
[0043] S2, preparing tea polyphenol nano-selenium: adding 0.2 g of sodium selenite to 50 mL of the tea polyphenol solution, and incubating the mixture in a water bath at 50° C. for 4 h to obtain tea polyphenol nano-selenium particles.
[0044] Example 3
[0045] A method for preparing tea polyphenol nano-selenium comprises the following steps:
[0046] Preparation of tea polyphenols: Weigh tea powder and use methanol with a concentration of 100% to extract tea polyphenols through a water bath, remove the supernatant solution, and obtain a tea polyphenol solution. The specific method is as follows:
[0047] S1, crush the green tea "Chunbo Green" into tea powder, pass through an 80-mesh sieve, weigh 1g (accurate to 0.0001g) of tea powder into a 50mL centrifuge tube, add 25mL of 70% methanol aqueous solution preheated at 70℃, stir well with a glass to moisten, immediately transfer to a 70℃ water bath for 10min (stir once every 5min), cool to room temperature after leaching, centrifuge at 3500r / min for 10min, and transfer the supernatant to a 50mL volumetric flask. The residue is extracted once with 25mL of 70% methanol aqueous solution, and the above operation is repeated. Combine the extracts to make up to 50mL, shake well, filter with a 0.45μm membrane, and obtain a tea polyphenol solution for standby use (the extract can be stored at 4℃ for up to 24h).
[0048] S2, preparing tea polyphenol nano-selenium: adding 0.3 g of sodium selenite to 50 mL of the tea polyphenol solution, and incubating the mixture in a water bath at 50° C. for 4 h to obtain tea polyphenol nano-selenium particles.
[0049] Example 4
[0050] A method for preparing tea polyphenol nano-selenium comprises the following steps:
[0051] Preparation of tea polyphenols: Weigh tea powder and use methanol with a concentration of 100% to extract tea polyphenols through a water bath, remove the supernatant solution, and obtain a tea polyphenol solution. The specific method is as follows:
[0052] S1, crush the green tea "Chunbo Green" into tea powder, pass through an 80-mesh sieve, weigh 1g (accurate to 0.0001g) of tea powder into a 50mL centrifuge tube, add 25mL of 70% methanol aqueous solution preheated at 70℃, stir well with a glass to moisten, immediately transfer to a 70℃ water bath for 10min (stir once every 5min), cool to room temperature after leaching, centrifuge at 3500r / min for 10min, and transfer the supernatant to a 50mL volumetric flask. The residue is extracted once with 25mL of 70% methanol aqueous solution, and the above operation is repeated. Combine the extracts to make up to 50mL, shake well, filter with a 0.45μm membrane, and obtain a tea polyphenol solution for standby use (the extract can be stored at 4℃ for up to 24h).
[0053] S2, preparing tea polyphenol nano-selenium: adding 0.4 g of sodium selenite to 50 mL of the tea polyphenol solution, and incubating the mixture in a water bath at 50° C. for 4 h to obtain tea polyphenol nano-selenium particles.
[0054] Example 5
[0055] A method for preparing tea polyphenol nano-selenium comprises the following steps:
[0056] Preparation of tea polyphenols: Weigh tea powder and use methanol with a concentration of 100% to extract tea polyphenols through a water bath, remove the supernatant solution, and obtain a tea polyphenol solution. The specific method is as follows:
[0057] S1, crush the green tea "Chunbo Green" into tea powder, pass through an 80-mesh sieve, weigh 1g (accurate to 0.0001g) of tea powder into a 50mL centrifuge tube, add 25mL of 70% methanol aqueous solution preheated at 70℃, stir well with a glass to moisten, immediately transfer to a 70℃ water bath for 10min (stir once every 5min), cool to room temperature after leaching, centrifuge at 3500r / min for 10min, and transfer the supernatant to a 50mL volumetric flask. The residue is extracted once with 25mL of 70% methanol aqueous solution, and the above operation is repeated. Combine the extracts to make up to 50mL, shake well, filter with a 0.45μm membrane, and obtain a tea polyphenol solution for standby use (the extract can be stored at 4℃ for up to 24h).
[0058] S2, preparing tea polyphenol nano-selenium: adding 0.5 g of sodium selenite to 50 mL of the tea polyphenol solution, and incubating the mixture in a water bath at 50° C. for 4 h to obtain tea polyphenol nano-selenium particles.
[0059] Example 6
[0060] A method for preparing tea polyphenol nano-selenium comprises the following steps:
[0061] Preparation of tea polyphenols: Weigh tea powder and use methanol with a concentration of 100% to extract tea polyphenols through a water bath, remove the supernatant solution, and obtain a tea polyphenol solution. The specific method is as follows:
[0062] S1, crush the green tea "Chunbo Green" into tea powder, pass through an 80-mesh sieve, weigh 1g (accurate to 0.0001g) of tea powder into a 50mL centrifuge tube, add 25mL of 70% methanol aqueous solution preheated at 70℃, stir well with a glass to moisten, immediately transfer to a 70℃ water bath for 10min (stir once every 5min), cool to room temperature after leaching, centrifuge at 3500r / min for 10min, and transfer the supernatant to a 50mL volumetric flask. The residue is extracted once with 25mL of 70% methanol aqueous solution, and the above operation is repeated. Combine the extracts to make up to 50mL, shake well, filter with a 0.45μm membrane, and obtain a tea polyphenol solution for standby use (the extract can be stored at 4℃ for up to 24h).
[0063] S2, preparing tea polyphenol nano-selenium: adding 0.6 g of sodium selenite to 50 mL of the tea polyphenol solution, and incubating the mixture in a water bath at 50° C. for 4 h to obtain tea polyphenol nano-selenium particles.
[0064] 2. Characterization and stability test of the prepared tea polyphenol nano-selenium:
[0065] (1) Use a particle size analyzer to measure the particle size and potential of tea polyphenol nanoselenium.
[0066] (2) Calculation of selenium conversion rate: The Se 4+ The concentration is then converted into selenium conversion rate. The selenium conversion rate conversion formula is shown below.
[0067] Selenium conversion rate conversion formula: Selenium conversion rate = (converted into Se by adding sodium selenite concentration 4+ Concentration - Se measured by atomic fluorescence 4+ concentration) / converted to Se by adding sodium selenite concentration 4+ Concentration (total selenium concentration) × 100%
[0068] (3) Total antioxidant capacity: The total antioxidant capacity (T-AOC) detection kit (ABTS microplate method) (manufacturer: Yuanye, catalog number: R24146-300T) was used to determine its ability to scavenge ABTS.
[0069] (4) Storage stability: The storage stability of GTP-SeNPs was determined by measuring the particle size of GTP-SeNPs stored at 4°C for 48 days.
[0070] (5) Temperature stability: GTP-SeNPs and aqueous solutions were placed in a sealed tube and then immersed in water at different temperatures (4°C, 25°C, 50°C, 70°C, and 90°C) for 1 h. The particle size was measured after cooling to room temperature to measure its temperature stability.
[0071] (6) pH stability: The pH of the GTP-SeNPs samples was adjusted to 3, 5, 7, 9, and 11 with 0.1 M hydrochloric acid or sodium hydroxide and left for 1 h. The size of the particles was then determined to analyze their pH stability.
[0072] (7) Ion concentration stability: To study the effect of ion concentration on its stability, equal amounts of NaCl / KCl / CaCl2 / MgCl2 / ZnCl2 / FeCl2 solutions (50, 100, 150, and 200 mM) were added to the GTP-SeNPs liquid sample. After mixing well and standing for 1 h, the particle size was measured to determine its stability.
[0073] Determination of Nano-Selenium Content in Tea Polyphenols:
[0074] Phenol-sulfuric acid method for total sugar determination: the method is carried out in accordance with "GB / T 15672-2009 Determination of total sugar content in edible fungi".
[0075] Determination of polyphenols by Folin phenol method: The method refers to "4 Detection of tea polyphenols in tea" in "GB / T 8313-2018 Determination of tea polyphenols and catechins in tea" for the determination of polyphenols.
[0076] 3. Characterization Results
[0077] (1) Stability
[0078] The screening conditions were: particle size, potential, selenium conversion rate and total antioxidant capacity. Finally, 0.5g sodium selenite / 50mL tea polyphenol solution was screened out.
[0079] like Figure 2 As shown, during the preparation process, 0.1 g, 0.2 g, 0.3 g, 0.4 g, 0.5 g, and 0.6 g of sodium selenite were added respectively, and the stability of the prepared tea polyphenol nano-selenium was measured.
[0080] like Figure 2 As shown in the figure, the particle size, potential, selenium conversion rate and total antioxidant capacity of the prepared tea polyphenol nano-selenium were tested by adding 0.1g, 0.2g, 0.3g, 0.4g, 0.5g and 0.6g of sodium selenite respectively during the preparation process. The results show that the screening conditions of small particle size, high absolute value of potential, high selenium conversion rate and strong total antioxidant capacity are screened, and the best result is obtained by adding 0.5g sodium selenite / 50mL tea polyphenol solution.
[0081] Figure 3 to Figure 5 The stability of tea polyphenol nano-selenium particles at different temperatures, different pH values and after storage for 48 days.
[0082] The analysis is as follows: Tea polyphenols-SeNPs have good temperature and pH stability, among which the temperature stability is better than the pH. There are only differences in temperature stability at 50℃ and 70℃, and the others are relatively stable.
[0083] As for pH, the stability is not very good, and the particle size shows a significant upward trend with the increase of pH.
[0084] 48-day storage stability: Tea polyphenol nano-selenium is not very stable from 0 to 18 days. Starting from the 24th day, the particle size of tea polyphenol nano-selenium tends to be stable, and its potential tends to be stable after one month.
[0085] Tea polyphenols-SeNPs have good stability to monovalent ions.
[0086] According to the particle size potential results, the stability of tea polyphenols-SeNPs to divalent ions is analyzed as follows: Figure 6 to Figure 11 As shown:
[0087] For Ca 2+, tea polyphenols-SeNPs were not tolerated.
[0088] For Mg 2+ , tea polyphenol-SeNPs tolerate low concentrations (50mM) but not high concentrations (≥100mM)
[0089] For Zn 2+ , tea polyphenols-SeNPs are not tolerated.
[0090] For Fe 2+ , tea polyphenols-SeNPs tolerate low concentrations (50mM) but not high concentrations (≥100mM) (tea polyphenols-SeNPs have poor stability to divalent ions. This may be because divalent ions can bind to nano-selenium and increase its particle size.)
[0091] For Na + According to the particle size results, the stability is good. According to the potential results, it is found that tea polyphenol-SeNPs are more stable at low ion concentration (50mM-100mM).
[0092] For K + According to the particle size results, the stability is good. According to the potential results, it is found that tea polyphenol-SeNPs have poor stability at low ion concentration (50mM) and high ion concentration (200mM).
[0093] Application Examples
[0094] Application of tea polyphenol nano-selenium in adsorption or removal of aluminum ions
[0095] Standard tubes: Take 7 25mL stoppered colorimetric tubes and add 0.500mL, 1.00mL, 1.50mL, 2.00mL, 2.50mL and 3.00mL of 1mg / L aluminum standard solution respectively (the masses of aluminum in this series of standard solutions are 0.500μg, 1.00μg, 1.50μg, 2.00μg, 2.50μg and 3.00μg respectively), and add water to the 10mL mark.
[0096] Sample tube:
[0097] Take 6 25mL stoppered colorimetric tubes, add 0.20mL of 10mg / L aluminum standard solution (the mass of aluminum in this series of solutions is 2.00μg), then add 5.00mL, 6mL, 7mL, 8mL, 9mL, and 10mL of tea polyphenol nano-selenium respectively, centrifuge at 8000rpm for 20min, take the supernatant, and add water to make up to 10mL mark.
[0098] Take 6 25mL stoppered colorimetric tubes, add 0.500mL, 1.00mL, 1.50mL, 2.00mL, 2.50mL and 3.00mL of 10mg / L aluminum standard solution respectively (the masses of aluminum in this series of solutions are 0.500μg, 1.00μg, 1.50μg, 2.00μg, 2.50μg, 3.00μg respectively), add 9mL of tea polyphenol nano-selenium respectively, centrifuge at 8000rpm for 20min, take the supernatant, and add water to make up to 10mL mark.
[0099] Reagent blank tube: Pipette 1.00 mL of blank solution (water) into a 25 mL stoppered colorimetric tube and add water to the 10 mL mark.
[0100] Add 1 drop of p-nitrophenol ethanol solution (1g / L) to the above-mentioned standard tube, sample tube, and reagent blank tube, mix well, add ammonia solution (1+1) until it turns light yellow, add nitric acid solution (2.5%) until the yellow color just disappears, add 1mL more, add 1mL ascorbic acid solution (10g / L), mix well, add 3mL chrome azuro blue S solution (1g / L), mix well, add 1mL TritonX-100 solution (3%), 3mL CPB solution (3g / L), 3mL ethylenediamine-hydrochloric acid buffer solution, add water to make up to 25.0mL, mix well, and let stand for 40min.
[0101] At a wavelength of 620nm, use a 1cm cuvette to measure the absorbance value with a blank solution as a reference. Use the mass of aluminum in the standard series solution as the horizontal coordinate and the corresponding absorbance value as the vertical coordinate to draw a standard curve. Quantify by comparing the absorbance value of the sample solution with the standard curve.
[0102] The results are as follows Fig.12 As shown, with the increase of selenium content, tea polyphenol nanoselenium scavenged Al 3+ The capacity shows a trend of increasing first and then decreasing, reaching a maximum of about 60%. 3+ The content of tea polyphenol nano-selenium increased, and the removal of Al 3+ The capacity showed a significant downward trend. 2μg Al 3+ After 4.109×10 -4 After the reaction of tea polyphenol nanoselenium with gSe content is completed, Al 3+ The final content was 0.78 μg.
[0103] Although the preferred embodiments of the present invention have been described, those skilled in the art may make other changes and modifications to these embodiments once they have learned the basic creative concept. Therefore, the appended claims are intended to be interpreted as including the preferred embodiments and all changes and modifications that fall within the scope of the present invention.
[0104] Obviously, those skilled in the art can make various changes and modifications to the present invention without departing from the spirit and scope of the present invention. Thus, if these modifications and variations of the present invention fall within the scope of the claims of the present invention and their equivalents, the present invention is also intended to include these modifications and variations.
Claims
1. A method for preparing tea polyphenol nano-selenium particles, characterized in that: The following steps are involved: Tea polyphenols and SeO3 2- The source is used as the raw material for the reduction reaction, and SeO3 2- Converted into nano-Se to obtain tea polyphenol nano-selenium particles.
2. The preparation method according to claim 1, characterized in that: Add SeO3 to the tea polyphenol solution 2- The substance is subjected to reduction reaction at 45°C to 55°C for 3 to 5 hours to obtain tea polyphenol nano-selenium particles.
3. The preparation method according to claim 2, characterized in that: The SeO3 2- The substance is sodium selenite, the concentration of the tea polyphenol solution is 2.5-3.0 g / L, and the mass ratio of the sodium selenite to the tea polyphenol solution is 1:0.22-0.
34.
4. The preparation method according to claim 1, characterized in that: The tea polyphenol solution is specifically prepared by mixing green tea powder with a methanol solution having a volume fraction of 65% to 75%, extracting at 65° C. to 75° C. for 8 to 12 minutes, collecting the extract, and filtering to obtain the tea polyphenol solution.
5. The preparation method according to claim 4, characterized in that: The mass volume ratio of the green tea powder and the methanol solution is 1g:40mL-60mL.
6. The preparation method according to claim 4, characterized in that: The extraction is performed 1 to 3 times.
7. The preparation method according to claim 1, characterized in that: The particle size of the tea polyphenol nano-selenium is 205.573nm-227.027nm.
8. Tea polyphenol nano-selenium particles prepared by the preparation method according to any one of claims 1 to 7.
9. Use of the tea polyphenol nano-selenium particles according to claim 8 in removing aluminum ions from wastewater.