CN115520905A - MoS 2 /CoS 2 Preparation method and application of heterostructure nanoenzyme - Google Patents
MoS 2 /CoS 2 Preparation method and application of heterostructure nanoenzyme Download PDFInfo
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Abstract
The invention relates to MoS 2 /CoS 2 The preparation method of heterostructure nano enzyme and its application are characterized by that firstly, in KSCN, co (NO) is added respectively 3 ·6H 2 O and (NH) 4 ) 6 Mo 7 O 24 ·4H 2 O, fully stirring to ensure that the components are fully mixed; then placing the mixture into a muffle furnace, heating and standing the mixture, obtaining a compact solid solution after the reaction is finished, and dissolving the compact solid solution by using deionized water; then using a large amount of deionized water and BWashing and filtering the mixture with alcohol for multiple times to remove excess KSCN; finally drying in vacuum to obtain MoS 2 /CoS 2 . MoS in the invention 2 /CoS 2 The heterostructure nanoenzyme can be reacted with H 2 O 2 Synergistically effective in killing drug-resistant bacteria while avoiding high concentrations of H 2 O 2 In the material and in low concentrations of H 2 O 2 Under the synergistic effect of the components, the antibacterial agent has excellent antibacterial performance on gram-positive bacteria and gram-negative bacteria; the heterojunction nano enzyme can be applied to the fields of treating bacterial infection and wound healing.
Description
Technical Field
The invention belongs to the field of biological and medical sterilization, and particularly relates to MoS 2 /CoS 2 Preparation method and application of heterostructure nanoenzyme are provided.
Background
The nanometer enzyme is a nanometer material with enzyme-like activity, and can be widely applied to the fields of biosensors, antibiosis, disease treatment and the like. At present, a large number of nanomaterials have been demonstrated to contain multiple activities such as one or more of oxidase, peroxidase, and catalase, broadly classified as including metal oxide/sulfide, metal organic framework, and monoatomic. Transition Metal Sulfides (TMSs), e.g. MoS 2 CoxSy and NiSx, because of their unique biological, chemical and physical properties, are finding increasing application to the field of catalysis by many scientists. However, TMSs have problems of insufficient active sites, poor stability, etc., resulting in insufficient catalytic performance for the intended purpose.
Therefore, in recent years, a great deal of research has been conducted to improve catalytic performance by controlling the morphology, composition of the heterogeneous interface, and other strategies. The charge rearrangement in the heterogeneous heterostructure can be reasonably regulated and controlled through the electronegativity difference between different sulfides and the charge transfer between the 3d orbit and the S2p orbit of different transition metals, so that the electron transfer is accelerated, the internal electric field effect is excited, and the catalytic activity and the reaction kinetics of the nanoenzyme are obviously improved. The interface engineering can be used as a channel or an intermediate for electron transfer among different components, can optimize and adjust the electronic structure of the catalyst, and plays an important role in improving the catalytic performance.
In recent years, diseases caused by pathogenic bacteria account for one third of the death number of the world every year, seriously threaten human life, and are still global public health problems. Particularly, as the drug-resistant bacteria and even superbacteria appear due to unreasonable use of antibiotics, methicillin-resistant staphylococcus aureus (MRSA) as a typical superbacteria has strong drug resistance to methicillin, amoxicillin, penicillin, oxacillin and many other common antibiotics, and MRSA infected wounds can develop into serious systemic infection such as sepsis if not treated timely or treated improperly, and then can induce the function failure of organs of the body, even threaten the life of patients. The treatment of infected wounds is difficult due to the strong drug resistance of MRSA, so that the problem which is troubled by the medical and scientific communities at present is urgently solved. Therefore, it is of great importance to develop novel materials with broad-spectrum antibacterial properties.
Therefore, the invention designs a MoS 2 /CoS 2 A heterostructure nanoenzyme.
Disclosure of Invention
In order to solve the technical problem, the invention designs the MoS 2 /CoS 2 Preparation method and application of heterostructure nanoenzyme, moS 2 /CoS 2 The heterostructure nanoenzyme can be reacted with H 2 O 2 Synergistically effective in killing drug-resistant bacteria while avoiding high concentrations of H 2 O 2 In the material and in low concentrations of H 2 O 2 Under the synergistic effect of the components, the antibacterial agent has excellent antibacterial performance on gram-positive bacteria and gram-negative bacteria; the heterojunction nano enzyme can be applied to the fields of treating bacterial infection and wound healing.
In order to achieve the technical effects, the invention is realized by the following technical scheme: moS 2 /CoS 2 Heterojunction nanoThe preparation method of the rice enzyme specifically comprises the following steps:
s1, adding Co (NO) into KSCN 3 ·6H 2 O and (NH) 4 ) 6 Mo 7 O 24 ·4H 2 O, fully stirring to fully mix the components;
s2, placing the mixture into a muffle furnace, heating and standing the mixture, obtaining a compact solid solution after the reaction is finished, and dissolving the compact solid solution with deionized water;
s3, washing and filtering the mixture for multiple times by using a large amount of deionized water and ethanol to remove redundant KSCN;
s4, drying in vacuum to obtain MoS 2 /CoS 2 。
Further, the S1 specifically includes: in the range of 20g KSCN, 0.8g Co (NO) was added 3 ·6H 2 O and 0.1g (NH) 4 ) 6 Mo 7 O 24 ·4H 2 And O, fully stirring to fully mix the components.
Further, the S2 specifically includes: putting the solid solution into a muffle furnace, heating to 300 ℃, standing for 2h at the temperature of 5 ℃/min, obtaining a compact solid solution after the reaction is finished, and dissolving the solid solution by using deionized water.
Further, the S4 specifically includes: vacuum drying at 80 deg.C overnight to obtain MoS 2 /CoS 2 。
Further, the MoS prepared by the preparation method 2 /CoS 2 A heterojunction nanoenzyme.
Further from the above, said a MoS 2 /CoS 2 Application of heterojunction nanoenzyme in inhibiting kanamycin-resistant escherichia coli and methicillin-resistant staphylococcus aureus.
The invention has the beneficial effects that:
(1) The preparation method of the heterojunction nanoenzyme is simple, does not need complex instruments and equipment, has low cost and is expected to be used for industrial production.
(2) The invention adopts nano enzyme as bactericide and adopts nano enzyme to kill bacteria at low concentration H 2 O 2 In the presence of the compound, the ROS with strong toxicity to bacteria can be rapidly and effectively generated,it can effectively inhibit the growth of bacteria, has broad-spectrum bactericidal property, has lower toxicity to normal cells, and does not have the problem of bacterial drug resistance.
(3) Compared with the prior sterilization technology, the nano enzyme is a heterojunction material prepared by a salt solution method, and can catalyze H 2 O 2 Decomposing into ROS with super strong sterilization capability, and combining the synergistic catalytic effect between the bimetallic sulfides, the catalytic action of the nano enzyme is greatly enhanced, and the purpose of high-efficiency sterilization is achieved.
(4) The nano enzyme bactericide based on the heterojunction is used as a dressing of an inorganic nano material, and can be used for promoting the bacteriostasis and healing of the wound of a mouse infected with methicillin-resistant staphylococcus aureus.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings used in the description of the embodiments will be briefly introduced below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and it is obvious for those skilled in the art that other drawings can be obtained according to the drawings without creative efforts.
FIG. 1 is the present invention MoS 2 /CoS 2 XRD spectrum of the heterostructure;
FIG. 2 is a MoS of the present invention 2 、CoS 2 、MoS 2 /CoS 2 NFs scanning electron microscope, transmission electron microscope, X-ray energy dispersion spectrum, element mapping images; wherein (A) MoS 2 、(B)CoS 2 、(C)MoS 2 /CoS 2 NFs are SEM images; (D) MoS 2 、(E)CoS 2 、(F)MoS 2 /CoS 2 NFs are HRTEM images; (G) MoS 2 /CoS 2 NFs is EDS picture; (H) is an element map;
FIG. 3 is a MoS of the present invention 2 /CoS 2 Schematic in vitro antibacterial activity of NFs; wherein (A) CoS is added into gram-negative bacteria (kanamycin-resistant Escherichia coli) and gram-positive bacteria (methicillin-resistant Staphylococcus aureus) 2 、MoS 2 、MoS 2 /CoS 2 NFs and H 2 O 2 The latter image; (B) For adding CoS 2 、MoS 2 、MoS 2 /CoS 2 NFs and H 2 O 2 The bacterial growth curve graph is obtained after 24 h;
FIG. 4 is a photograph of wounds of mice infected with Staphylococcus aureus treated at different times and with different treatments; (B) relative wound sizes of mice after different treatments.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
MoS 2 /CoS 2 The preparation method of the heterojunction nanoenzyme specifically comprises the following steps:
s1, adding Co (NO) into KSCN 3 ·6H 2 O and (NH) 4 )6Mo 7 O 24 ·4H 2 O, fully stirring to fully mix the components;
s2, placing the solid solution into a muffle furnace, heating and standing the solid solution, obtaining a compact solid solution after the reaction is finished, and dissolving the compact solid solution by using deionized water;
s3, washing and filtering the mixture for multiple times by using a large amount of deionized water and ethanol to remove redundant KSCN;
s4, drying in vacuum to obtain MoS 2 /CoS 2 。
The S1 specifically comprises: in the range of 20g KSCN, 0.8g Co (NO) was added 3 ·6H 2 O and 0.1g (NH) 4 )6Mo 7 O 24 ·4H 2 And O, fully stirring to fully mix the components.
The S2 specifically comprises: putting the solid solution into a muffle furnace, heating to 300 ℃, standing for 2h at the temperature of 5 ℃/min, obtaining a compact solid solution after the reaction is finished, and dissolving the solid solution by using deionized water.
The S4 specifically comprises: vacuum drying at 80 deg.C overnight to obtain MoS 2 /CoS 2 。
Further, moS prepared by the preparation method 2 /CoS 2 A heterojunction nanoenzyme.
Example 2
As shown in fig. 1 to 4, further from the above, a MoS 2 /CoS 2 The application of the heterojunction nanoenzyme in inhibiting kanamycin-resistant escherichia coli and methicillin-resistant staphylococcus aureus is as follows:
(1) Methicillin-resistant Staphylococcus aureus (337371) and kanamycin-resistant Escherichia coli (186761) and the corresponding MDR isolates serve as the main models for gram-positive (G +) and gram-negative (G-) bacteria, respectively. The activated bacteria were cultured in about 50mL of Luria-Bertani (LB) liquid medium. Incubating the mixture for 24 hours at 37 ℃ and 150r/min in a constant-temperature incubator to obtain bacterial suspension, and evaluating the antibacterial performance of the bacterial suspension by a plate counting method.
The specific operation is as follows: diluting the prepared bacterial suspension to 1 × 10 -5 CFU/mL, 50. Mu.L of the bacterial suspension was mixed with MoS 2 /CoS 2 And H 2 O 2 (50. Mu.L, 0.5 mM) were mixed. Shaking in a constant temperature incubator (37 deg.C, 150 r/min) for 2h. The mixed sample was then coated on LB solid medium. Finally, standing and culturing for 24h in an incubator, and observing and counting the number of colonies. The bacterial growth curve was measured by adding physiological saline as a blank. Mixing the bacteria with MoS 2 /CoS 2 In the presence or absence of H 2 O 2 Co-culturing in the system, and measuring the Optical Density (OD) of the bacterial suspension every 2h 600nm )。
(2) 100. Mu.L of medium + 50. Mu.L of bacteria (group 1), 50. Mu.L of medium + 50. Mu.L of bacteria + 50. Mu.L of MoS 2 /CoS 2 (2 mg/mL) (group 2), 50. Mu.L of Medium + 50. Mu.LH 2 O 2 (0.5 mM) + 50. Mu.L of bacterial solution (group 3), 50. Mu.L of LH 2 O 2 (0.5 mM) + 50. Mu.L of bacterial solution + 50. Mu.L of MoS 2 /CoS 2 (2 mg/mL) (group 4).
(3) Sterilization rate = (number of control colony-number of experimental colony)/number of control colony x 100%
(4) Firstly, establishing a mouse wound surface carrier model, carrying out intraperitoneal injection on an anesthetized mouse by using 10% chloral hydrate solution of 1 mu L/g, depilating after anesthesia, and disinfecting the skin of a depilated area by using iodophor and 75% alcohol. A round wound with a diameter of 40mm was made with medical scissors on the back of the mouse to the full skin. 20 μ L (concentration about 10) of freshly prepared methicillin-resistant Staphylococcus aureus suspension was taken 5 CFU/mL) is dripped into the wound surface; after the wound surface model was established, mice were divided into 8 groups and MoS was assigned 2 、 CoS 2 And MoS 2 /CoS 2 Dripping the suspension on the wound surface of a mouse infected by methicillin-resistant staphylococcus aureus according to the dosage of 10 mu L, and then adding 2.5mM H on the wound surface 2 O 2 Solution 10. Mu.L (without addition of H) 2 O 2 In place of physiological saline). Mice wound healing was observed and photographed daily.
Example 3
As shown in fig. 1 to 4, in MoS 2 /CoS 2 In (c), only all obvious CoS 2 Diffraction peaks are all inverted, and MoS 2 /CoS 2 MoS is not seen in NFs 2 Corresponding diffraction peak, which may be MoS 2 Completely uniformly dispersed in CoS 2 A surface.
From FIG. 2A, moS 2 Is a flower-like structure composed of smooth nanosheets, and CoS 2 The morphology of (2B) exhibits a hexagonal structure. For MoS 2 /CoS 2 It can be seen that MoS is well maintained 2 The nanoflower surface of (2) shows a large number of honeycomb-shaped cavities at the same time (fig. 2C). By determining MoS in HRTEM image 2 And CoS 2 Further defining the formation of a heterointerface. MoS 2 Has a lattice spacing of 0.62nm and is a 002 crystal plane (FIG. 2D). At the same time, co 3 S 4 CoS of 2 And (311) the lattice spacings of the (200) and (210) planes of the plane are 0.28, 0.25 and 0.28nm, respectively (FIG. 2E). In MoS 2 /CoS 2 In-plane spacing of 0.28 and 0.57nm respectively belong to CoS 2 (211) Crystal face and MoS 2 And a sharp interface is formed between the two crystal planes as shown by the yellow line in fig. 2F. (002) Of (2) plane crystalThe spacing between the cells is about 0.57nm, slightly smaller than the original MoS 2 (0.62 nm), this is represented by MoS 2 And CoS 2 Are produced by strong interactions. This appearance includes rich nano-interfaces at the atomic level and subtle lattice distortions that provide more highly active sites to bind the oxidation substrate and thereby optimize catalytic performance. FIGS. 2G and 2H are MoS, respectively 2 /CoS 2 X-ray energy dispersion spectra and elemental maps demonstrating MoS 2 /CoS 2 The elements Mo, co and S of NFs are uniformly dispersed in the flower-like structure.
As shown in FIG. 3A, we observed MoS 2 、CoS 2 、H 2 O 2 And H alone 2 O 2 Processing MoS 2 Or CoS 2 After this time, the number of bacterial colonies did not change significantly, but H was added 2 O 2 MoS of (1) 2 /CoS 2 Thereafter, the survival rate of each bacterium was significantly decreased, H 2 O 2 To MoS 2 /CoS 2 The antibacterial rate of NFs can reach 99%. To further verify MoS 2 /CoS 2 The growth curve of the bacteria in 24H after adding the nanoenzyme was measured by kanamycin-resistant Escherichia coli (FIG. 3B), and it can be clearly seen that in H 2 O 2 Addition of MoS 2 /CoS 2 Bacteria at OD within 24 hours after NFs 600nm There was little significant change in UV absorption, which also indicates that MoS 2 /CoS 2 NFs have good antimicrobial properties.
In view of MoS 2 /CoS 2 NFs nanocatalysts have good in vitro antibacterial properties and we performed in vivo evaluations to determine their potential in wound healing. The KM mice with wounds on the back were divided into 8 groups. Then, use 10 5 CFU mL -1 The methicillin-resistant staphylococcus aureus cells of (a) are used to prepare a bacterially infected wound. After 1 day of infection, different treatments (physiological saline, moS) were injected on the wound surface every day 2 、CoS 2 、MoS 2 /CoS 2 、H 2 O 2 、MoS 2 +H 2 O 2 、CoS 2 +H 2 O 2 And MoS 2 /CoS 2 +H 2 O 2 ) And photographed. FIG. 4A shows MoS 2 /CoS 2 +H 2 O 2 The group healed significantly faster than the other controls. MoS 2 /CoS 2 +H 2 O 2 The wound of the treated mice gradually scabbed and basically healed after 9d of injection. Notably, moS compared to the control group 2 /CoS 2 +H 2 O 2 The healing process was significantly accelerated (fig. 4B and 4C).
In the description herein, references to the description of "one embodiment," "an example," "a specific example," etc., mean that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the invention. In this specification, the schematic representations of the terms used above do not necessarily refer to the same embodiment or example. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples.
The preferred embodiments of the invention disclosed above are intended to be illustrative only. The preferred embodiments are not intended to be exhaustive or to limit the invention to the precise embodiments disclosed. Obviously, many modifications and variations are possible in light of the above teaching. The embodiments were chosen and described in order to best explain the principles of the invention and the practical application, to thereby enable others skilled in the art to best utilize the invention. The invention is limited only by the claims and their full scope and equivalents.
Claims (6)
1. MoS 2 /CoS 2 The preparation method of the heterojunction nanoenzyme is characterized by comprising the following steps:
s1, adding Co (NO) into KSCN 3 ·6H 2 O and (NH) 4 ) 6 Mo 7 O 24 ·4H 2 O, fully stirring to fully mix the components;
s2, placing the mixture into a muffle furnace, heating and standing the mixture, obtaining a compact solid solution after the reaction is finished, and dissolving the compact solid solution with deionized water;
s3, washing and filtering the mixture for multiple times by using a large amount of deionized water and ethanol to remove redundant KSCN;
s4, drying in vacuum to obtain MoS 2 /CoS 2 。
2. MoS according to claim 1 2 /CoS 2 The preparation method of the heterojunction nanoenzyme is characterized in that the S1 specifically comprises the following steps: in the range of 20g KSCN, 0.8g Co (NO) was added 3 ·6H 2 O and 0.1g (NH) 4 ) 6 Mo 7 O 24 ·4H 2 And O, fully stirring to fully mix.
3. A MoS according to claim 1 2 /CoS 2 The preparation method of the heterojunction nanoenzyme is characterized in that the S2 specifically comprises the following steps: placing the mixture into a muffle furnace, heating to 300 ℃, keeping stand for 2h at the temperature of 5 ℃/min, obtaining a compact solid solution after the reaction is finished, and dissolving the compact solid solution with deionized water.
4. A MoS according to claim 1 2 /CoS 2 The preparation method of the heterojunction nanoenzyme is characterized in that the S4 specifically comprises the following steps: vacuum drying at 80 deg.C overnight to obtain MoS 2 /CoS 2 。
5. MoS produced by the production method according to claims 1 to 4 2 /CoS 2 A heterojunction nanoenzyme.
6. MoS according to claim 5 2 /CoS 2 Application of heterojunction nano-enzyme in inhibiting kanamycin-resistant escherichia coli and methicillin-resistant staphylococcus aureus.
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| JIN WANG等: "CoS2/MoS2 Nanosheets with Enzymatic and Photocatalytic Properties for Bacterial Sterilization", ACS APPLIED NANO MATERIALS, vol. 4, pages 7698 - 7711 * |
| SONG HE等: "Low-temperature molten salt synthesis of Mos2@CoS2 heterostructures for efficient hydrogen evolution reaction", CHEMCOMM, vol. 56, no. 41, pages 5548 - 5551 * |
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