CN114532333B - Method for constructing attapulgite-zinc oxide nano composite antibacterial material by using liquorice extract - Google Patents

Method for constructing attapulgite-zinc oxide nano composite antibacterial material by using liquorice extract Download PDF

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CN114532333B
CN114532333B CN202210094355.6A CN202210094355A CN114532333B CN 114532333 B CN114532333 B CN 114532333B CN 202210094355 A CN202210094355 A CN 202210094355A CN 114532333 B CN114532333 B CN 114532333B
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attapulgite
zinc oxide
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CN114532333A (en
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杨芳芳
王爱勤
惠爱平
康玉茹
王晓梅
许江
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Lanzhou Institute of Chemical Physics LICP of CAS
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Abstract

The invention discloses a method for constructing an attapulgite-zinc oxide nano composite antibacterial material by using a liquorice extract, which comprises the steps of adding attapulgite and a zinc source into a liquorice water extract, adjusting the pH value by using sodium hydroxide, reacting for 30 to 150min under the conditions of stirring and oil bath at the constant temperature of 55 to 95 ℃, centrifuging, washing and drying the obtained product, thus obtaining the zinc oxide/attapulgite composite antibacterial material. The attapulgite-zinc oxide composite material is constructed by a one-step method by using water as a solvent, natural attapulgite as a carrier and a liquorice aqueous extract as a reducing agent and a stabilizing agent, and has strong antibacterial activity on gram-positive bacteria and gram-negative bacteria. The preparation method is simple and green, has mild reaction conditions and low cost, and is easy for mass production and preparation.

Description

Method for constructing attapulgite-zinc oxide nano composite antibacterial material by using liquorice extract
Technical Field
The invention belongs to the field of material synthesis, and particularly relates to a method for constructing an attapulgite-zinc oxide nano composite antibacterial material by using a liquorice extract.
Background
The wide use and abuse of antibiotics, particularly the large-scale application of the antibiotics to livestock and poultry breeding, cause a large amount of drug-resistant bacteria to appear, and cause great threat to human health, and a new method and a new strategy for solving the problem are urgently needed. The research and wide application of the nanometer technology bring revolutionary changes to the industrial and biomedical fields, people can design and construct materials on the nanometer scale, obtain higher-activity antibacterial materials, and is expected to replace antibiotics to resist bacterial infection.
Due to the high specific surface area and high reactivity, the metal and metal oxide nanoparticles can provide effective, targeted and broad-spectrum antibacterial activity in smaller dosage, and become a research hotspot in the antibacterial field. Among them, zinc oxide nanoparticles show wider usability due to their broad-spectrum antibacterial activity and good biocompatibility (chemical development: 2018, 37, 621, nano-Micro lett. 2015, 7, 219). However, the nano metal particles are easy to agglomerate due to the extremely high surface energy, and the biological activity of the nano metal particles is seriously influenced. The carrier loaded with zinc oxide nanoparticles can effectively prevent the nanoparticles from agglomerating, and the nanoparticles with uniform dispersibility can be obtained (CN 111067917A, CN103283781B, ACS appl. Mater. Interfaces 2014, 6, 2791). Attapulgite is a hydrous magnesium-rich aluminosilicate clay mineral with a chain layered structure, and is widely applied to petroleum, chemical engineering, building materials, papermaking, medicines, agriculture and other aspects due to unique physicochemical properties and process performance. Due to the nanorod crystal structure, high specific surface area and surface silicon hydroxyl group of the attapulgite, the attapulgite becomes an ideal carrier for loading inorganic nanoparticles.
The traditional method for synthesizing the zinc oxide nano material relates to the use of toxic chemical substances, the preparation cost is high, the generated by-products can cause negative effects on the environment, and toxic substances can also remain on the surface of the obtained product, so that the nano material has high biotoxicity. In recent years, a green synthesis method based on biological resources has attracted great attention, and in particular, a plant extract is used as a medium for synthesizing nano materials (CN 202110676827.4, fine chemical engineering 2020, 37, 1793, chemico-biol. Interact. 2018, 286, 60). The method for preparing the zinc oxide nano material by the plant reduction mainly utilizes biomolecules such as protein, saccharide, polyphenol, flavone and the like which are rich in plant extract to serve as a reducing agent and a protective agent, and reduces metal ions under mild conditions. As only natural plant extract is used in the process, no chemical reagent is added, and the reaction condition is mild. Therefore, compared with the traditional preparation method, the plant reduction method has the advantages of environmental protection, mild reaction conditions, low cost, wide and easily available raw materials and the like, so that the plant reduction method is considered as an ideal route capable of replacing the traditional preparation method.
Licorice is an ancient and commonly used Chinese herbal medicine. The licorice extract contains compounds such as saponin, flavonoid, terpenoid, polysaccharide and the like, has biological effects of resisting virus, resisting inflammation, resisting oxidation, resisting bacteria and the like, and is widely applied to prevention and treatment of diseases of human and animals (modern agricultural science and technology).
2019, 3, 211). Research shows that bioactive substances in liquorice extract have the effects of reducing and stabilizing metal nanoparticles (int. J.biol. Macro. 2020, 141, 422), and are currently used for preparing nanoparticles of titanium dioxide, silver, gold, zinc and the like, but the development of attapulgite loaded zinc oxide antibacterial materials is not reported.
Disclosure of Invention
The invention aims to provide a method for constructing an attapulgite-zinc oxide nano composite antibacterial material by using a liquorice extract, which can effectively avoid the generation of toxic byproducts by adopting the liquorice extract as a medium, and the synthesized nano material has high safety, excellent antibacterial performance and easy large-scale production.
1. Preparation of attapulgite-zinc oxide nano composite antibacterial material
The method for constructing the attapulgite-zinc oxide nano composite antibacterial material by using the liquorice extract adopts water as a solvent, natural attapulgite as a carrier and the liquorice aqueous extract as a reducing agent and a stabilizing agent, and the attapulgite-zinc oxide composite material is constructed by a one-step method, and has strong antibacterial activity on gram-positive bacteria and gram-negative bacteria. The preparation method is simple and green, has mild reaction conditions and low cost, and is easy for mass production and preparation. The method specifically comprises the following steps:
1) Adding the licorice powder into distilled water under stirring, stirring at 70-85 ℃ for 60-100min, and filtering to obtain a licorice extract solution. Wherein the mass concentration of the licorice powder in distilled water is 10 to 50 percent.
2) Respectively adding attapulgite powder and zinc salt into a liquorice extract solution, stirring and dispersing uniformly, and then adding a sodium hydroxide solution to adjust the pH to 7 to 11 to obtain a precursor mixed solution; wherein the zinc salt is at least one of zinc nitrate hexahydrate, zinc sulfate heptahydrate and zinc acetate dihydrate, and the concentration of the zinc salt is 0.02 to 0.2mol/L; the mass ratio of the attapulgite powder to the zinc salt is 20 to 1.
3) Reacting the precursor mixed solution for 30 to 150min under the conditions of stirring and oil bath at the constant temperature of 55 to 95 ℃, centrifuging, washing and drying the obtained product to obtain the zinc oxide/attapulgite composite antibacterial material; the stirring speed of the precursor mixed solution is 300 to 600rpm.
The synthesis mechanism of the invention is as follows: the licorice extract contains flavonoid, saponin, terpenoid, polysaccharide and other phytochemicals, and the substances are used for reducing metal ions and stabilizing nano particles to obtain nano zinc oxide with smaller size.
FIG. 1 is SEM atlas of the attapulgite-zinc oxide nano composite antibacterial material prepared by the invention, which shows that spherical zinc oxide nano particles with the diameter of about 10-30nm are loaded on the surface of the attapulgite, and XRD in FIG. 2 further shows that the attapulgite-zinc oxide nano composite material is successfully prepared by the invention. From the FTIR spectrum of FIG. 3, it was found that the peak intensity was at 2975cm -1 And 2364cm -1 Shows absorption peaks of methyl and hydroxyl groups at 3423cm -1 The absorption peak is shifted, which shows that flavonoid, saponin, terpenoid and polysaccharide in the licorice extract all participate in the reduction of the zinc oxide nano-particles. The molecular structure of these materials contains a large number of polar hydroxyl groups, and the electron-rich oxygen atoms contained in them can react with electropositive metal cations. Meanwhile, amino and carboxyl in the active molecules have better affinity with zinc oxide nano-particles and are attached to the surfaces of the particles to prevent the particles from agglomerating and growingLarge, and then obtaining zinc oxide nano-particles with smaller size.
2. Antibacterial property of attapulgite-zinc oxide nano composite antibacterial material
The antibacterial performance of the attapulgite-zinc oxide nano composite antibacterial material prepared by the invention is evaluated by testing the Minimum Inhibitory Concentration (MIC) by adopting an agar dilution method, and the testing steps are as follows:
(1) Preparing a bacterial suspension: thawing a standard strain stored at-20 ℃, inoculating the standard strain to an LB culture medium, and placing the standard strain into a shaking incubator to culture for 12 hours under the conditions of 160rpm and 37 ℃; then, the bacterial liquid and the fresh culture medium are mixed according to the ratio of 1: mixing the materials according to the volume ratio of 100, inoculating the mixture into an LB culture medium again, and culturing for 3 hours under the same condition; finally, taking the strains to prepare 10 4 CFU/mL of bacterial suspension.
(2) Sample plate preparation: and dispersing the sterilized samples to be detected into an agar culture medium which is dissolved and cooled to 40-50 ℃ according to different concentrations, and cooling to obtain a sample plate.
(3) Inoculating bacterial liquid and culturing: sucking fresh bacterial suspension prepared in 1-2 muL (1), and inoculating the fresh bacterial suspension to 3 different positions of the sample flat plate in the step (2); inoculating bacterial suspension into the agar plate without a sample as a positive control, and taking the agar plate without an antibacterial sample and without the bacterial suspension as a negative control; and (3) placing the inoculated plate in an incubator at 37 ℃ and culturing for 18-24h.
(4) And (4) analyzing results: bacteria were considered to be completely inhibited if no colony grew at all in the sample plates after completion of the incubation, wherein the minimum sample concentration to completely inhibit bacterial growth was the MIC. The MIC of the attapulgite-zinc oxide nanocomposite antibacterial material in examples 1-5 for Escherichia coli and Staphylococcus aureus is shown in Table 1, which shows that the attapulgite-zinc oxide nanocomposite prepared by the invention has excellent antibacterial activity.
TABLE 1 MIC (mg/mL) for Attapulgite-Zinc oxide nanocomposites in examples 1-5 for E.coli and Staphylococcus aureus
Figure 785809DEST_PATH_IMAGE001
In conclusion, the method for constructing the attapulgite-zinc oxide nano composite antibacterial material by using the liquorice extract in a mediated manner has the following advantages:
1. the natural attapulgite is used as a carrier, and the generation process of the zinc oxide nano-particles is regulated and controlled, so that the particle agglomeration can be effectively controlled, and a nano-material with higher activity is obtained;
2. the method has the advantages of simple process, low cost, no environmental pollution, good stability of the obtained nano material, high biocompatibility and antibacterial activity, and environmental friendliness, and is a synthesis process suitable for large-scale production.
Drawings
FIG. 1 is an SEM image of an attapulgite-zinc oxide nanocomposite prepared in example 4 of the invention;
FIG. 2 is an XRD diagram of the attapulgite-zinc oxide nanocomposite prepared in example 4 of the invention;
FIG. 3 is an FTIR chart of the attapulgite-zinc oxide nanocomposite prepared in example 4 of the present invention;
FIG. 4 is a UV-vis diagram of the attapulgite-zinc oxide nanocomposite prepared in examples 1-5 of the present invention;
FIG. 5 is a diagram showing the antibacterial effect of the attapulgite-zinc oxide nanocomposite prepared in examples 1-5 of the present invention.
Detailed Description
The method for constructing attapulgite-zinc oxide nano composite antibacterial material by using licorice extract of the invention is explained in detail by the following specific examples.
Example 1
(1) Adding 10g Glycyrrhrizae radix powder into 100mL distilled water under stirring, stirring at 85 deg.C for 60min, and filtering to obtain Glycyrrhrizae radix extract solution;
(2) Weighing 3g of attapulgite powder and 0.53g of zinc sulfate heptahydrate, respectively adding into 100mL of liquorice extract solution, stirring and dispersing uniformly, and then dropwise adding 2mol/L sodium hydroxide to adjust the pH to 10 to obtain precursor mixed solution;
(3) And (3) reacting the precursor solution for 150min under the conditions of mechanical stirring at 500rpm and constant-temperature oil bath at 55 ℃, centrifuging, washing for three times and drying the obtained product to obtain the zinc oxide/attapulgite composite antibacterial material, wherein the MICs (minimum inhibitory concentration) on escherichia coli and staphylococcus aureus are shown in Table 1.
Example 2
(1) Adding 20g Glycyrrhrizae radix powder into 100mL distilled water under stirring, stirring at 75 deg.C for 90min, and filtering to obtain Glycyrrhrizae radix extract solution;
(2) Weighing 3g of attapulgite powder and 1.1g of zinc acetate dihydrate, respectively adding into 100mL of the licorice extract solution, stirring and dispersing uniformly, and then dropwise adding 2mol/L sodium hydroxide to adjust the pH to 8, thereby obtaining precursor mixed solution;
(3) And (3) reacting the precursor solution for 45min under the conditions of mechanical stirring at 300rpm and constant-temperature oil bath at 80 ℃, centrifuging, washing for three times and drying the obtained product to obtain the zinc oxide/attapulgite composite antibacterial material, wherein the MICs (minimum inhibitory concentration) on escherichia coli and staphylococcus aureus are shown in Table 1.
Example 3
(1) Adding 30g Glycyrrhrizae radix powder into 100mL distilled water under stirring, stirring at 80 deg.C for 90min, and filtering to obtain Glycyrrhrizae radix extract;
(2) Weighing 3g of attapulgite powder and 1.6g of zinc acetate dihydrate, respectively adding into 100mL of licorice extract solution, stirring and dispersing uniformly, and then dropwise adding 2mol/L sodium hydroxide solution to adjust the pH value to 11 to obtain precursor mixed solution;
(3) And (3) reacting the precursor solution for 60min under the conditions of mechanical stirring at 600rpm and constant-temperature oil bath at 70 ℃, centrifuging, washing for three times and drying the obtained product to obtain the zinc oxide/attapulgite composite antibacterial material, wherein the MICs (minimum inhibitory concentration) on escherichia coli and staphylococcus aureus are shown in Table 1.
Example 4
(1) Adding 40g Glycyrrhrizae radix powder into 100mL distilled water under stirring, stirring at 70 deg.C for 100min, and filtering to obtain Glycyrrhrizae radix extract solution;
(2) Weighing 3g of attapulgite powder and 2.97g of zinc nitrate hexahydrate, respectively adding into 100mL of liquorice extract solution, stirring and dispersing uniformly, and then dropwise adding 2mol/L sodium hydroxide to adjust the pH to 9 to obtain precursor mixed solution;
(3) And (3) reacting the precursor solution for 90min under the conditions of mechanical stirring at 400rpm and constant-temperature oil bath at 60 ℃, centrifuging, washing for three times and drying the obtained product to obtain the zinc oxide/attapulgite composite antibacterial material, wherein the MICs (minimum inhibitory concentration) on escherichia coli and staphylococcus aureus are shown in Table 1.
Example 5
(1) Adding 50g Glycyrrhrizae radix powder into 100mL distilled water under stirring, stirring at 80 deg.C for 100min, and filtering to obtain Glycyrrhrizae radix extract solution;
(2) Weighing 3g of attapulgite powder and 5.5g of zinc nitrate hexahydrate, respectively adding into 100mL of liquorice extract solution, stirring and dispersing uniformly, and then dropwise adding 2mol/L sodium hydroxide to adjust the pH to 7 to obtain precursor mixed solution;
(3) And (3) reacting the precursor solution for 30min under the conditions of mechanical stirring at 600rpm and constant-temperature oil bath at 95 ℃, centrifuging, washing for three times and drying the obtained product to obtain the zinc oxide/attapulgite composite antibacterial material, wherein the MICs (minimum inhibitory concentration) on escherichia coli and staphylococcus aureus are shown in Table 1.

Claims (3)

1. A method for constructing an attapulgite-zinc oxide nano composite antibacterial material by using a liquorice extract is characterized by comprising the following steps:
1) Adding the licorice powder into distilled water under stirring, stirring at 70-85 ℃ for 60-100min, and filtering to obtain a licorice extract solution;
2) Respectively adding attapulgite powder and zinc salt into a liquorice extract solution, stirring and dispersing uniformly, and then adding a sodium hydroxide solution to adjust the pH to 7 to 11 to obtain a precursor mixed solution; the zinc salt is at least one of zinc nitrate hexahydrate, zinc sulfate heptahydrate and zinc acetate dihydrate, and the concentration of the zinc salt in the licorice extract solution is 0.02 to 0.2mol/L; the mass ratio of the attapulgite powder to the zinc salt is 20 to 1;
3) And (3) reacting the precursor mixed solution for 30 to 150min under the conditions of stirring and oil bath at the constant temperature of 55 to 95 ℃, centrifuging, washing and drying the obtained product to obtain the zinc oxide/attapulgite composite antibacterial material.
2. The method for constructing the attapulgite-zinc oxide nano composite antibacterial material by using the licorice extract according to claim 1, wherein the method comprises the following steps: in the step 1), the mass concentration of the licorice powder in distilled water is 10 to 50%.
3. The method for constructing the attapulgite-zinc oxide nano composite antibacterial material by using the licorice extract according to claim 1, wherein the method comprises the following steps: in the step 3), the stirring speed of the precursor mixed liquid is 300 to 600rpm.
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