CN112846220A - Method for synthesizing nano-silver based on alfalfa extract - Google Patents
Method for synthesizing nano-silver based on alfalfa extract Download PDFInfo
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- CN112846220A CN112846220A CN202110028843.2A CN202110028843A CN112846220A CN 112846220 A CN112846220 A CN 112846220A CN 202110028843 A CN202110028843 A CN 202110028843A CN 112846220 A CN112846220 A CN 112846220A
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- 241000219823 Medicago Species 0.000 title claims abstract description 52
- 235000017587 Medicago sativa ssp. sativa Nutrition 0.000 title claims abstract description 52
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 title claims abstract description 34
- 238000000034 method Methods 0.000 title claims abstract description 28
- 239000000284 extract Substances 0.000 title claims abstract description 24
- 230000002194 synthesizing effect Effects 0.000 title claims abstract description 17
- 238000006243 chemical reaction Methods 0.000 claims abstract description 19
- 235000012054 meals Nutrition 0.000 claims abstract description 17
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 16
- GAMYVSCDDLXAQW-AOIWZFSPSA-N Thermopsosid Natural products O(C)c1c(O)ccc(C=2Oc3c(c(O)cc(O[C@H]4[C@H](O)[C@@H](O)[C@H](O)[C@H](CO)O4)c3)C(=O)C=2)c1 GAMYVSCDDLXAQW-AOIWZFSPSA-N 0.000 claims abstract description 14
- 229930003944 flavone Natural products 0.000 claims abstract description 14
- 150000002212 flavone derivatives Chemical class 0.000 claims abstract description 14
- 235000011949 flavones Nutrition 0.000 claims abstract description 14
- VHBFFQKBGNRLFZ-UHFFFAOYSA-N vitamin p Natural products O1C2=CC=CC=C2C(=O)C=C1C1=CC=CC=C1 VHBFFQKBGNRLFZ-UHFFFAOYSA-N 0.000 claims abstract description 14
- 238000001035 drying Methods 0.000 claims abstract description 9
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(I) nitrate Inorganic materials [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 claims abstract description 8
- 238000002156 mixing Methods 0.000 claims abstract description 6
- 239000000843 powder Substances 0.000 claims abstract description 6
- 238000002791 soaking Methods 0.000 claims abstract description 6
- 230000017260 vegetative to reproductive phase transition of meristem Effects 0.000 claims abstract description 6
- 102000004190 Enzymes Human genes 0.000 claims abstract description 4
- 108090000790 Enzymes Proteins 0.000 claims abstract description 4
- 238000001914 filtration Methods 0.000 claims abstract description 4
- 238000003306 harvesting Methods 0.000 claims abstract description 4
- 238000007873 sieving Methods 0.000 claims abstract description 3
- 238000012360 testing method Methods 0.000 claims description 11
- 229930003935 flavonoid Natural products 0.000 claims description 10
- 150000002215 flavonoids Chemical class 0.000 claims description 10
- 235000017173 flavonoids Nutrition 0.000 claims description 10
- 244000025254 Cannabis sativa Species 0.000 claims description 7
- 101710134784 Agnoprotein Proteins 0.000 claims description 5
- 239000007788 liquid Substances 0.000 claims description 3
- 239000002244 precipitate Substances 0.000 claims description 3
- 238000003756 stirring Methods 0.000 claims description 3
- 238000001291 vacuum drying Methods 0.000 claims description 3
- 238000007789 sealing Methods 0.000 claims 1
- 238000002360 preparation method Methods 0.000 abstract description 6
- 240000004658 Medicago sativa Species 0.000 abstract description 3
- 230000007613 environmental effect Effects 0.000 abstract description 3
- 239000002245 particle Substances 0.000 abstract description 3
- 235000010624 Medicago sativa Nutrition 0.000 abstract description 2
- 239000000654 additive Substances 0.000 abstract description 2
- 230000000996 additive effect Effects 0.000 abstract description 2
- 238000004519 manufacturing process Methods 0.000 abstract description 2
- 241000220286 Sedum Species 0.000 abstract 1
- 238000010521 absorption reaction Methods 0.000 description 4
- 230000015572 biosynthetic process Effects 0.000 description 4
- 238000003786 synthesis reaction Methods 0.000 description 4
- 241000196324 Embryophyta Species 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 238000011160 research Methods 0.000 description 3
- 239000003153 chemical reaction reagent Substances 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 230000018109 developmental process Effects 0.000 description 2
- 239000002105 nanoparticle Substances 0.000 description 2
- 238000000053 physical method Methods 0.000 description 2
- 239000000419 plant extract Substances 0.000 description 2
- 230000009467 reduction Effects 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000002137 ultrasound extraction Methods 0.000 description 2
- 241000220485 Fabaceae Species 0.000 description 1
- 238000000862 absorption spectrum Methods 0.000 description 1
- 239000013543 active substance Substances 0.000 description 1
- 229930013930 alkaloid Natural products 0.000 description 1
- 150000003797 alkaloid derivatives Chemical class 0.000 description 1
- 239000003963 antioxidant agent Substances 0.000 description 1
- 230000003078 antioxidant effect Effects 0.000 description 1
- 235000006708 antioxidants Nutrition 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003638 chemical reducing agent Substances 0.000 description 1
- 230000009849 deactivation Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000007865 diluting Methods 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 239000013067 intermediate product Substances 0.000 description 1
- 229910021645 metal ion Inorganic materials 0.000 description 1
- 230000000813 microbial effect Effects 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 150000007524 organic acids Chemical class 0.000 description 1
- 150000008442 polyphenolic compounds Chemical class 0.000 description 1
- 235000013824 polyphenols Nutrition 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 239000003223 protective agent Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000001308 synthesis method Methods 0.000 description 1
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/16—Making metallic powder or suspensions thereof using chemical processes
- B22F9/18—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
- B22F9/24—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from liquid metal compounds, e.g. solutions
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
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- Chemical & Material Sciences (AREA)
- Nanotechnology (AREA)
- Physics & Mathematics (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
- General Physics & Mathematics (AREA)
- Manufacturing & Machinery (AREA)
- Crystallography & Structural Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Cultivation Of Plants (AREA)
Abstract
The invention discloses a method for synthesizing nano-silver based on alfalfa extract, which comprises the following steps: harvesting overground parts of the last flowering stage of the No. 10 Sedum Medicago sativa, deactivating enzymes for 30min at 105 ℃, drying for 1-2 d at 65 ℃, crushing by using a crusher, sieving by using a 60-mesh sieve to obtain alfalfa powder, and storing in a room-temperature sealed bag; soaking 1g of alfalfa meal in ethanol at room temperature for 30-60 min, and reacting for 10-30 min under the ultrasonic reaction condition. Filtering at normal temperature to fix the volume to 50 mL; mixing AgNO3Mixing with herba Medicaginis total flavone extractive solution at volume ratio of 1:2 at 450rpm under normal temperature and in dark for 30min, and standing at normal temperature in dark for 1-3 days to obtain herba Medicaginis total flavone extractive solution with particle size of about 50 nm. The preparation process has the advantages of low production cost, environmental protection, mild reaction conditions, no need of any additive in the reaction process and the like.
Description
Technical Field
The invention belongs to the technical field of nano-silver synthesis, and relates to a method for synthesizing nano-silver based on an alfalfa extract.
Background
With the continuous development of nano technology, the synthesis methods of nano silver are more and more, and the preparation method of nano silver can be divided into a chemical method, a physical method, a microbial reduction method and a plant extract reduction method according to the preparation principle and method of nano silver. In the chemical preparation process, the used reducing agent and protective agent have serious pollution to the environment; in the physical method, although the purity of the obtained nano silver is high, the method has high requirements on equipment and high operation cost and energy requirement. Therefore, scientific research institutions search two green and environment-friendly methods, which have the advantages of low production cost, environmental friendliness, mild reaction conditions, no need of any additive in the reaction process and the like.
Alfalfa (Medicago sativa L.) is a perennial herb of the genus Medicago of the family Leguminosae, and has been reputed as the king of pasture. The overground plant of the alfalfa contains a large amount of active substances (such as polyphenol, flavonoid, organic acid, alkaloid and other antioxidant ingredients), so that the flavonoid extract of the alfalfa can be used for reducing metal ions and wrapping stably generated nano particles to form green nano particles.
The method for synthesizing the nano-silver by utilizing the alfalfa extract has high safety and strong operability, and the nano-silver synthesized by reducing the plant extract has the characteristics of mild reaction conditions, simplicity in operation, low cost and the like. At present, the research on the synthesis of nano-silver by using the alfalfa extract is few in China, and the invention synthesizes nano-silver by using the alfalfa total flavone extract.
Disclosure of Invention
The invention aims to overcome the defects in the prior art and provides a method for synthesizing nano-silver based on an alfalfa extract, wherein the alfalfa extract used in the method is Sedi No. 10, which is alfalfa introduced from Bai Green (Tianjin) International grass industries, Inc. of animal husbandry and veterinary institute of agricultural academy of sciences in Fujian province. The method comprises the steps of planting the seedlings in test fields of grassy scientific test bases in northschool district of the northwest agriculture and forestry science and technology university of Yangxi city of Shaanxi province, and harvesting overground plant parts at the late flowering stage of the seedlings.
AgNO for use in the invention3The reagent is from AR (analytical grade) of juong corporation.
The technical scheme of the invention is as follows: the nano-silver is synthesized by extracting the total flavone from the overground part of the alfalfa, and the process comprises the steps of preparing the alfalfa powder, extracting the total flavone from the grass powder by ultrasonic waves, and synthesizing the total flavone into the nano-silver.
The specific technical scheme is as follows:
a method for synthesizing nano-silver based on alfalfa extract comprises the following steps:
(1) preparing alfalfa meal: harvesting overground parts of the alfalfa at the late flowering stage of the Sedi No. 10 alfalfa in a test field of a grassy scientific test base in the northwest school district of the northwest agriculture and forestry science and technology university of Yangling district of Yanyang city of Shaanxi province, deactivating enzyme for 30min at 105 ℃, drying for 1-2 d at 65 ℃, crushing by using a crusher, sieving by using a 60-mesh sieve to obtain alfalfa powder, and storing in a room-temperature sealed bag;
(2) extracting total flavonoids in grass meal by ultrasonic waves: firstly, 1g of the alfalfa meal in the step (1) is taken to be soaked in 60% ethanol with the feed liquid ratio of 1:30(g/mL) for 30-60 min at room temperature, and then the alfalfa meal is reacted for 10-30 min under the ultrasonic reaction condition of the temperature of 40-50 ℃ and the power of 40 Khz. After the ultrasonic reaction, filtering with filter paper at normal temperature, fixing the volume to 50mL with 60% ethanol in a volumetric flask, and storing at 4 ℃ for later use;
(3) synthesizing nano-silver by using total flavonoids: mixing AgNO3And (3) mixing the alfalfa total flavone extract extracted in the step (2) with the alfalfa total flavone extract extracted in the step (2) according to the volume ratio of 1:2, stirring at 450rpm at normal temperature in a dark place for 30min, and standing at normal temperature in a dark place for 1-3 d. And centrifuging the reacted solution at 12000rpm at normal temperature to obtain a brownish black precipitate, performing vacuum drying in a drying dish for 24 hours, and storing at room temperature in a dark place.
Preferably, in step (1), drying is performed for 2 d.
Preferably, in the step (2), soaking is carried out for 60min, and then reaction is carried out for 30min under the ultrasonic reaction condition of 50 ℃ and 40Khz power.
Preferably, the concentration of total flavonoids extracted in step (2) is 0.035 mg/mL.
Preferably, in step (3), the mixture is left in the dark for 3 d.
Preferably, in the step (3), AgNO is used3The concentration was 2 mmol/L.
Compared with the prior art, the invention has the beneficial effects that:
the invention has the advantages of synthesizing the nano silver: the nano silver prepared by the method has an absorption peak at 400nm, has the particle size of about 50nm, has the advantages of safety, simplicity, environmental protection and the like, adopts low energy consumption for intermediate reaction, does not generate intermediate products harmful to the environment, and is combined with the sustainable development and the green chemistry advocated by the state.
Drawings
FIG. 1 is an image of a nano-silver solution prepared in example 3 of the method of the present invention under a projection electron microscope;
FIG. 2 is an absorption peak image of a nano-silver solution prepared in example 3 of the method of the present invention under an ultraviolet spectrophotometer;
FIG. 3 is an image of the absorption peaks of the nanosilver solution and the alfalfa total flavone extract prepared in example 3 of the method of the present invention under the Fourier infrared absorption spectrum.
Detailed Description
The technical solution of the present invention will be described in further detail with reference to the accompanying drawings and specific embodiments.
The alfalfa variety used in the invention is Sedi No. 10, which is introduced from Bai Green (Tianjin) International grass industry Co., Ltd by animal husbandry and veterinary research institute of agricultural academy of sciences in Fujian province. The overground part of the terminal flowering stage of the test field is harvested in the test field of the grassy scientific test base in the northwest school district of the university of agriculture and forestry, science and technology, northwest of Yanyang city, Shaanxi province.
AgNO for use in the invention3The reagent is from AR (analytical grade) of juong corporation.
Example 1 preparation of alfalfa meal
In a test field of a grassy scientific test base in the northwest school district of the university of agriculture and forestry, science and technology, Yangxing, Shanxi, Yanyang, Yangling, Yangxing, the overground plant part of the alfalfa at the late flowering stage, which is of the variety 'Saidi No. 10', is harvested, the alfalfa is de-enzymed in an oven at 105 ℃ for 30min, the alfalfa is dried at 65 ℃ for 1-2 d, crushed by a crusher, sieved by a 60-mesh sieve, and the alfalfa powder is obtained and stored in a room-temperature sealed bag.
Example 2 ultrasonic extraction of Total Flavonoids in grass meal
Taking 1g of the alfalfa meal, soaking the alfalfa meal in 60% ethanol with the feed liquid ratio of 1:30(g/mL) for 30-60 min at room temperature, and then reacting for 10-30 min under the ultrasonic reaction condition of 40-50 ℃ and 40kHz power. After the ultrasonic reaction, filtering with filter paper at normal temperature, diluting to 50mL with 60% ethanol in a volumetric flask, and storing at 4 ℃ for later use.
Example 3 Synthesis of Nano silver from Total Flavonoids
Mixing AgNO3And stirring the extract and the extracted alfalfa total flavone extract for 30min at normal temperature and in the dark at the rotating speed of 450rpm according to the volume ratio of 1:2, and standing for 1-3 d in the dark at normal temperature. And centrifuging the reacted solution at 12000rpm at normal temperature to obtain a brownish black precipitate, performing vacuum drying in a drying dish for 24 hours, and storing at room temperature in a dark place.
In the preparation of the alfalfa meal, after deactivation of enzymes for 30min, drying is carried out for 2d at 65 ℃.
The ultrasonic extraction of total flavone from grass meal is carried out by soaking in 60% ethanol for 60min, and reacting at 50 deg.C under ultrasonic reaction condition for 30 min. The total flavone concentration extracted according to this procedure was 0.035 mg/mL.
AgNO used in synthesis of nano-silver by using total flavonoids3The concentration is 2mmol/L, and the solution is protected from light for 3 days at normal temperature.
As shown in figures 1-3, the nano-silver prepared by the method has a particle size of about 50nm, an absorption peak at 400nm, and the periphery of the nano-silver is coated by total flavonoids.
The above description is only a preferred embodiment of the present invention, and the scope of the present invention is not limited thereto, and any simple modifications or equivalent substitutions of the technical solutions that can be obviously obtained by those skilled in the art within the technical scope of the present invention are within the scope of the present invention.
Claims (6)
1. A method for synthesizing nano-silver based on alfalfa extract is characterized by comprising the following steps:
(1) preparing alfalfa meal: harvesting overground parts of the terminal flowering stage of No. 10 Sedi alfalfa in a test field of a grassy scientific test base in the northwest school district of the northwest agriculture and forestry science and technology university of Yangling district of Yanyang city, Shanxi province, deactivating enzyme for 30min at 105 ℃, drying for 1-2 d at 65 ℃, crushing by using a crusher, sieving by using a 60-mesh sieve to obtain alfalfa powder, and storing in a room-temperature sealing bag;
(2) extracting total flavonoids in grass meal by ultrasonic waves: firstly, taking 1g of alfalfa meal in the step (1), soaking the alfalfa meal in 60% ethanol with a material-liquid ratio of 1:30g/mL for 30-60 min at room temperature, then reacting for 10-30 min under the ultrasonic reaction condition of 40-50 ℃ and 40Khz power, filtering the alfalfa meal with filter paper at room temperature after the ultrasonic reaction, fixing the volume to 50mL with 60% ethanol in a volumetric flask, and storing the alfalfa meal at 4 ℃ for later use;
(3) synthesizing nano-silver by using total flavonoids: mixing AgNO3And (3) stirring the alfalfa total flavone extract extracted in the step (2) for 30min at normal temperature and in the dark at the rotating speed of 450rpm according to the volume ratio of 1:2, standing for 1-3 d in the dark at normal temperature, centrifuging the solution after reaction at 12000rpm at normal temperature to obtain a brownish black precipitate, performing vacuum drying in a drying dish for 24h, and storing in the dark at room temperature.
2. The method for synthesizing nano silver based on the alfalfa extract as claimed in claim 1, wherein in step (1), the drying is performed for 2 d.
3. The method for synthesizing nano silver based on the alfalfa extract according to claim 1, wherein in the step (2), the soaking is performed for 60min, and then the reaction is performed for 30min under the ultrasonic reaction condition of 50 ℃ and 40Khz power.
4. The method for synthesizing nano silver based on alfalfa extract as claimed in claim 1, wherein the total flavone concentration extracted in step (2) is 0.035 mg/mL.
5. The method for synthesizing nano silver based on the alfalfa extract according to claim 1, wherein in step (3), the alfalfa extract is kept away from light for 3 days.
6. The method for synthesizing nano silver based on alfalfa extract as claimed in claim 1, wherein in step (3), AgNO is used3The concentration was 2 mmol/L.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN113996800A (en) * | 2021-10-28 | 2022-02-01 | 广东省科学院微生物研究所(广东省微生物分析检测中心) | Method for preparing nano-silver based on gynura bicolor extract |
| CN114769611A (en) * | 2022-04-06 | 2022-07-22 | 电子科技大学中山学院 | Method for preparing nano-silver by utilizing pine needle extract |
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