CN113305299A - Method for green preparation of silver nanoparticles by cooperation of hesperidin and pectin and application of silver nanoparticles - Google Patents
Method for green preparation of silver nanoparticles by cooperation of hesperidin and pectin and application of silver nanoparticles Download PDFInfo
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- CN113305299A CN113305299A CN202110683042.XA CN202110683042A CN113305299A CN 113305299 A CN113305299 A CN 113305299A CN 202110683042 A CN202110683042 A CN 202110683042A CN 113305299 A CN113305299 A CN 113305299A
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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
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- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
- A01N59/00—Biocides, pest repellants or attractants, or plant growth regulators containing elements or inorganic compounds
- A01N59/16—Heavy metals; Compounds thereof
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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
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/05—Metallic powder characterised by the size or surface area of the particles
- B22F1/054—Nanosized particles
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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
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/06—Metallic powder characterised by the shape of the particles
- B22F1/065—Spherical particles
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- 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
Abstract
The invention discloses a method for green preparation of silver nanoparticles by using hesperidin in cooperation with pectin and application thereof, which comprises the following specific steps: (1) preparing silver nitrate solution and sodium hydroxide solution; (2) accurately weighing a mixture of hesperidin and pectin according to the ratio of 3: 1-1: 3, adding a sodium hydroxide solution, and placing in a conical flask to form the hesperidin-pectin alkali solution. Placing the mixture in a microwave oven for assisting dissolution; (3) adding a silver nitrate solution into the solution, shaking up, putting into a microwave oven for microwave-assisted reaction, and standing; (4) the reaction conditions are selected according to the absorption peak value of about 400nm of ultraviolet light, and the liquid after the reaction is centrifuged at high speed. Taking the precipitate, adding a proper amount of distilled water, repeatedly centrifuging twice, and placing the precipitate in an oven to be dried overnight to obtain the silver nanoparticles. The preparation method has simple process and low cost, and the prepared product has the biological characteristics of nano-silver, such as broad-spectrum antibacterial activity, and also has the common biological activity of hesperidin and pectin.
Description
Technical Field
The invention belongs to the technical field of metal nanoparticle preparation, and particularly relates to a preparation method and application of a silver nanoparticle synthesized by cooperation of hesperidin and pectin.
Background
Due to outbreaks of infectious diseases caused by different pathogenic bacteria and deterioration of antibiotic resistance, there is an urgent need to find novel antibacterial agents having good safety and strong antibacterial activity to solve this problem. Nanoscale materials have now become novel antimicrobial agents due to their high surface area to volume ratio and their excellent chemical and physical properties. Silver nanoparticles (AgNPs) have proven to be a very effective antimicrobial agent, have the advantages of high biocompatibility, low toxicity, good membrane permeability, good optical surface properties, broad antimicrobial activity, etc., and have become the subject of the current research and wide application. It plays an important role in food, medicine, agriculture and many other fields. Because of its uniqueness and increasing availability.
At present, various methods for synthesizing silver nanoparticles have been developed, including chemical reduction methods, thermal decomposition methods, electrochemical methods, and the like, respectively. Terentva et al (2015) used various flavonoid compounds to successfully prepare silver nanoparticles, studied different bioactivities and antibacterial effects, and carried out partial characterization studies. Sobhan et al (2021) successfully prepared nano silver particles by using the Elaeagnus angustifolia Turcz extract, the obtained silver nanoparticles have high antibacterial effect, and the substances in the extract for effectively preparing the silver nanoparticles are proved to be pectin, flavonoid, polyphenol and the like. Su et al (2019) successfully prepared silver nanoparticles by a microwave-assisted method using pectin as a reducing agent and a stabilizer and silver nitrate as a precursor. The method is a green, efficient and economical method for preparing the silver nanoparticles. Song et al (2019) prepared uniform and stable curcumin silver nanocomposite particles by a simple sonication process using curcumin, which acts not only as a reducing agent but also as a stabilizing agent, and evaluated synergistic antimicrobial activity. These methods can successfully produce silver nanoparticles of varying size, shape, surface chemistry and charge, but generally involve the use of surfactants, reducing agents and hazardous chemicals. They often have a toxic and harmful effect on the environment and human health. In addition, various organic and inorganic substances are added to prevent aggregation of antibodies or control release of silver ions, thereby reducing antibacterial efficiency thereof. Therefore, it is also increasingly important to research a method for preparing nano silver in a green, nontoxic and simple manner and improving the antibacterial efficiency of the nano silver.
Therefore, researchers begin to use biological macromolecules or polymers as precursor substances, a new synthetic route based on the green chemical principle is provided, and hesperidin is adopted for co-preparation, so that the aim of increasing the antibacterial effect is fulfilled. Pectin is a natural polymer and macromolecular substance, has the characteristics of low toxicity, good biocompatibility, biodegradability, easy colloid formation and the like, and is an excellent biological material for preparing metal nanoparticles. Flavonoid compounds are a main category in natural extracts, are widely distributed in plants, and have various physiological functions. The flavonoid compound also has the advantages of biocompatibility, low toxicity, environmental friendliness and the like. Hesperidin is a representative bioactive compound among flavonoid compounds. Hesperidin is also a major dietary flavonoid, abundantly present in many citrus fruits and exhibits a wide range of biological properties. In addition, hesperidin is considered as an effective anti-inflammatory, anticancer and antioxidant drug, and it has a certain inhibitory effect on both gram-positive and gram-negative bacteria.
Researches show that the pectin is used as a reducing agent and a stabilizing agent to prepare the metal nano particles with excellent antibacterial performance, but the antibacterial performance of the metal nano particles needs to be further improved. The flavonoid compound hesperidin with good biological activity and a certain antibacterial effect can be used for preparing nano-silver together with pectin, so that the antibacterial performance of the nano-silver can be effectively improved.
Disclosure of Invention
The invention aims to solve the technical problem of a new idea for synthesizing silver nanoparticles by using hesperidin in cooperation with pectin. The silver nano particles are prepared by adding a flavonoid substance, namely hesperidin, into pectin, wherein the hesperidin is used as a reducing agent, and the pectin is used as a stabilizing agent, so that the antibacterial property of the pectin can be improved through the synergistic effect of the hesperidin and the pectin.
In order to solve the technical problems, the invention adopts the following technical scheme:
a method for green preparation of silver nanoparticles by cooperation of hesperidin and pectin comprises the following steps:
(1) preparing 0.1-0.7 mol/L silver nitrate solution and 1g/L sodium hydroxide solution;
(2) accurately weighing 0.2g of a mixture of hesperidin and pectin, wherein the ratio of pectin to hesperidin is 3: 1-1: 3, adding 100mL of sodium hydroxide solution, and placing in a 250mL conical flask to form a hesperidin-pectin alkali solution with the concentration of 1-3 mg/mL. Placing the mixture in a microwave oven, wherein the power is 400W, and dissolving for 1-3 min under the assistance of microwave;
(3) adding 2mL of silver nitrate solution into the solution, shaking up, putting into a microwave oven with the power of 100-800W, carrying out microwave-assisted reaction for 1-3 min, and standing for 10-30 min;
(4) the reaction conditions are selected according to the absorption peak value of ultraviolet light of about 400nm, and the liquid after reaction is centrifuged at high speed, wherein the rotating speed is 10000r/min, and the centrifuging time is 20 min. Taking the precipitate, adding a proper amount of distilled water, repeatedly centrifuging twice, and drying the precipitate in an oven at 50 ℃ overnight to obtain the silver nanoparticles.
The innovation points and advantages of the invention are as follows:
1. the invention uses hesperidin and pectin dissolved by alkali as a reducing agent and a stabilizing agent. Wherein the reducing agent is mainly hesperidin, and the stabilizer is mainly pectin. Reacting with silver nitrate to completely reduce silver ions into silver nano particles. Silver nano particles with better stability and better antibacterial performance are formed.
2. The preparation method of the silver nanoparticles adopts microwave-assisted synthesis of the silver nanoparticles, has simple preparation process, low cost and short reaction time, and avoids the use of toxic reducing agents.
3. The nano silver particles of the invention have wide biological activity, not only have the biological characteristics of nano silver such as broad-spectrum antibacterial activity, but also have the common biological activity of hesperidin and pectin. Therefore, the antibacterial material has wide application prospect as an efficient, low-cost and broad-spectrum antibacterial material, and can provide scientific basis for the research of medical antibacterial materials.
Drawings
FIG. 1 is a transmission electron micrograph (a) and a particle size distribution (b) of silver nanoparticles in example 1.
Fig. 2 is an ultraviolet-visible light absorption spectrum of the silver nanoparticles in example 1.
FIG. 3 is the absorbance of the silver nanoparticles of example 1 at a wavelength of 600nm for E.coli (a) and S.aureus (b) at different times.
Detailed Description
The invention is further described below with reference to the drawings and specific preferred embodiments of the description, without thereby limiting the scope of protection of the invention. The materials and equipment used in the following examples are commercially available.
The invention discloses a method for green preparation of silver nanoparticles by cooperation of hesperidin and pectin, which comprises the following steps:
the hesperidin and pectin dissolved by alkali are used as a reducing agent and a stabilizing agent, silver nanoparticles are synthesized by microwave assistance, and the nano silver particles are prepared by high-speed centrifugation. Overcomes the defects of the prior art, and provides a preparation method and application of the silver nanoparticles based on hesperidin and pectin, which are green, environment-friendly, low in toxicity, low in cost, high in yield and stronger in antibacterial activity.
Example 1
The embodiment is a method for preparing nano silver particles by using hesperidin in cooperation with pectin, and the method comprises the following steps of:
(1) accurately weighing 0.15g of hesperidin and 0.05g of pectin, adding 100mL of sodium hydroxide solution, and placing in a 250mL conical flask to form a hesperidin-pectin alkali solution with the concentration of 2 mg/mL;
(2) placing the obtained solution in a microwave oven, wherein the power is 400W, and carrying out microwave-assisted reaction for 2 min;
(3) dropwise adding 2mL of 0.5mol/L silver nitrate solution into the solution in the step (2), and uniformly stirring;
(4) putting the reaction reagent into a microwave oven with the power of 400W, heating for 2min, and standing for reaction for 20 min;
(5) centrifuging the reacted liquid at high speed under 10000r/min for 20min, collecting the precipitate, adding distilled water in equal amount, washing, and centrifuging twice;
(6) drying the precipitate product obtained in the step (5) at 50 ℃ overnight to obtain powder, namely nano silver particles;
(7) in an experiment, the reaction solution is changed from orange yellow transparent to brown black to show that silver nanoparticles are generated, ultraviolet spectrum scanning is carried out under the condition of the wavelength of 300-600 nm, and the maximum absorption peak near 400nm is used as an optimization condition;
(8) the silver nanoparticles obtained in this example were observed by a transmission electron microscope, the transmission electron microscope image of the silver nanoparticles is shown in fig. 1(a), the particle size distribution diagram is shown in fig. 1(b), and the average particle size of the silver nanoparticles prepared in this example is 14.9nm, and the silver nanoparticles are in a full sphere shape and have good dispersibility. Fig. 2 is an ultraviolet-visible light absorption spectrum of the prepared silver nanoparticles.
Example 2
This example is substantially the same as example 1, except that the ratio of the amount of hesperidin to pectin added (step (1)) is different, the total weight of hesperidin and pectin is 0.2g, and the ratio of hesperidin to pectin is 3: 1. 1: 1 and 1: 3.
example 3
This example was similar to example 1 except that the silver nitrate concentration (step (3)) was 0.1, 0.3, 0.5 and 0.7 mol/L.
Example 4
This example was similar to example 1, except that the standing time (step (4)) after the microwave reaction was 0, 10, 20 and 30min, respectively.
Example 5
The embodiment is a method for preparing silver nanoparticles by using hesperidin in cooperation with pectin in a green manner and application of the method in the field of bacteriostasis, and the silver nanoparticles obtained in the embodiment 1 are used for carrying out bacteriostasis experiments.
Experiment of minimum inhibitory concentration
3.2mg of the silver nanoparticle sample obtained in example 1 was weighed and dissolved in 1mL of broth to obtain 3.2 mg/mL. A series of concentration gradients were prepared for dilution of the stock solution in this way: 0mg/mL, 0.1mg/mL, 0.2mg/mL, 0.4mg/mL, 0.8mg/mL, 1.6mg/mL, 3.2 mg/mL.
0.2mL broth, 0.05mL nano-silver broth sample and 0.05mL Escherichia coli or Staphylococcus aureus suspension with the concentration controlled at 105About one/mL, and the mixture was mixed well and added to a cell culture 96-well plate, wherein the sample concentration in the system was 0. mu.g/mL, 16.7. mu.g/mL, 33.3. mu.g/mL, 66.7. mu.g/mL, 133.3. mu.g/mL, 266.7. mu.g/mL, and 533.3. mu.g/mL. Culturing for 0h, 3h, 6h, 9h, 12h, 15h and 24h, and detecting light absorption value (600nm) with microplate reader. The results are shown in FIG. 3, in which FIG. 3(a) is Escherichia coli, FIG. 3(b) is Staphylococcus aureus, the minimum inhibitory concentration of Escherichia coli is 66.7. mu.g/mL, and the minimum inhibitory concentration of Staphylococcus aureus is 133.3. mu.g/mL.
The above description is only a preferred embodiment of the present invention, and the protection scope of the present invention is not limited to the above-described embodiments. All technical schemes belonging to the idea of the invention belong to the protection scope of the invention. It should be noted that modifications and embellishments within the scope of the invention may be made by those skilled in the art without departing from the principle of the invention, and such modifications and embellishments should also be considered as within the scope of the invention.
Claims (6)
1. The method for preparing the silver nanoparticles in a green way by using the cooperation of hesperidin and pectin is characterized by comprising the following steps of:
(1) preparing a hesperidin-pectin alkali solution, accurately weighing hesperidin and pectin, dissolving by using a sodium hydroxide solution and dissolving by using microwave assistance to obtain the hesperidin-pectin alkali solution;
(2) adding a silver nitrate solution into the step 1;
(3) reacting the step 2 for a period of time under the assistance of microwaves;
(4) and (4) centrifuging the solution obtained in the step (3) at a high speed, and drying to obtain silver nanoparticles.
2. The method for green preparation of silver nanoparticles by using hesperidin in combination with pectin according to claim 1, wherein the hesperidin-pectin alkaline solution preparation method in the step is to accurately weigh a certain proportion of hesperidin and pectin, dissolve the hesperidin and the pectin by using a sodium hydroxide solution, and dissolve the hesperidin and the pectin by using microwave assistance to obtain the hesperidin-pectin alkaline solution.
3. The method for preparing silver nanoparticles in a green manner by using hesperidin in cooperation with pectin according to claim 1 is characterized in that a silver nitrate solution is prepared by dissolving a certain amount of silver nitrate in distilled water to prepare a silver nitrate solution with a concentration of 0.1-0.5 mol/L.
4. The method for green preparation of silver nanoparticles by using hesperidin in cooperation with pectin according to claim 1, wherein in the step, the microwave power is 0-800W, and the microwave time is 1-10 min.
5. The method for green preparation of silver nanoparticles by using hesperidin in cooperation with pectin according to claim 1, wherein in the step, the centrifugation time is 10-20 min.
6. The application of the hesperidin prepared by the preparation method of any one of claims 1-5 in cooperation with green preparation of the pectin to silver nanoparticles in the field of bacteriostasis.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113798506A (en) * | 2021-09-16 | 2021-12-17 | 云南省农业科学院热区生态农业研究所 | Preparation method of tamarind seed polysaccharide nano-silver |
| CN115058054A (en) * | 2022-07-17 | 2022-09-16 | 桂林理工大学 | Preparation method and application of nano-silver pectin composite sponge |
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2021
- 2021-06-21 CN CN202110683042.XA patent/CN113305299A/en not_active Withdrawn
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113798506A (en) * | 2021-09-16 | 2021-12-17 | 云南省农业科学院热区生态农业研究所 | Preparation method of tamarind seed polysaccharide nano-silver |
| CN115058054A (en) * | 2022-07-17 | 2022-09-16 | 桂林理工大学 | Preparation method and application of nano-silver pectin composite sponge |
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Application publication date: 20210827 |