CN114309636A - Chiral gold nano antibacterial material and preparation method thereof - Google Patents
Chiral gold nano antibacterial material and preparation method thereof Download PDFInfo
- Publication number
- CN114309636A CN114309636A CN202111633546.7A CN202111633546A CN114309636A CN 114309636 A CN114309636 A CN 114309636A CN 202111633546 A CN202111633546 A CN 202111633546A CN 114309636 A CN114309636 A CN 114309636A
- Authority
- CN
- China
- Prior art keywords
- solution
- chiral
- gold nano
- gold
- antibacterial material
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 title claims abstract description 92
- 239000010931 gold Substances 0.000 title claims abstract description 92
- 229910052737 gold Inorganic materials 0.000 title claims abstract description 89
- 239000000463 material Substances 0.000 title claims abstract description 33
- 230000000844 anti-bacterial effect Effects 0.000 title claims abstract description 27
- 238000002360 preparation method Methods 0.000 title claims abstract description 11
- 238000000034 method Methods 0.000 claims abstract description 14
- 239000000243 solution Substances 0.000 claims description 144
- CIWBSHSKHKDKBQ-JLAZNSOCSA-N Ascorbic acid Chemical compound OC[C@H](O)[C@H]1OC(=O)C(O)=C1O CIWBSHSKHKDKBQ-JLAZNSOCSA-N 0.000 claims description 40
- LZZYPRNAOMGNLH-UHFFFAOYSA-M Cetrimonium bromide Chemical compound [Br-].CCCCCCCCCCCCCCCC[N+](C)(C)C LZZYPRNAOMGNLH-UHFFFAOYSA-M 0.000 claims description 27
- 239000011668 ascorbic acid Substances 0.000 claims description 22
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims description 21
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 20
- 229960005070 ascorbic acid Drugs 0.000 claims description 20
- 235000010323 ascorbic acid Nutrition 0.000 claims description 20
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 claims description 20
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 14
- 108010016626 Dipeptides Proteins 0.000 claims description 13
- 229910004042 HAuCl4 Inorganic materials 0.000 claims description 13
- 239000007864 aqueous solution Substances 0.000 claims description 12
- 238000003756 stirring Methods 0.000 claims description 12
- 229910001961 silver nitrate Inorganic materials 0.000 claims description 10
- 238000002156 mixing Methods 0.000 claims description 8
- 238000010438 heat treatment Methods 0.000 claims description 6
- 239000003638 chemical reducing agent Substances 0.000 claims description 4
- 239000011259 mixed solution Substances 0.000 claims description 4
- 238000006243 chemical reaction Methods 0.000 claims description 3
- 239000002245 particle Substances 0.000 claims description 3
- 239000012279 sodium borohydride Substances 0.000 claims description 2
- 229910000033 sodium borohydride Inorganic materials 0.000 claims description 2
- 239000012467 final product Substances 0.000 claims 1
- 230000000694 effects Effects 0.000 abstract description 11
- 239000002086 nanomaterial Substances 0.000 abstract description 9
- 230000008859 change Effects 0.000 abstract description 2
- 230000001954 sterilising effect Effects 0.000 abstract description 2
- 230000005540 biological transmission Effects 0.000 abstract 1
- 239000003446 ligand Substances 0.000 abstract 1
- 238000004659 sterilization and disinfection Methods 0.000 abstract 1
- 241000894006 Bacteria Species 0.000 description 13
- 230000001580 bacterial effect Effects 0.000 description 8
- 239000000203 mixture Substances 0.000 description 8
- 241000191963 Staphylococcus epidermidis Species 0.000 description 7
- WOWHHFRSBJGXCM-UHFFFAOYSA-M cetyltrimethylammonium chloride Chemical compound [Cl-].CCCCCCCCCCCCCCCC[N+](C)(C)C WOWHHFRSBJGXCM-UHFFFAOYSA-M 0.000 description 6
- 206010040047 Sepsis Diseases 0.000 description 5
- 239000003921 oil Substances 0.000 description 5
- 239000002244 precipitate Substances 0.000 description 5
- 208000035143 Bacterial infection Diseases 0.000 description 3
- 208000022362 bacterial infectious disease Diseases 0.000 description 3
- 238000011156 evaluation Methods 0.000 description 3
- 208000015181 infectious disease Diseases 0.000 description 3
- 239000002082 metal nanoparticle Substances 0.000 description 3
- 230000004048 modification Effects 0.000 description 3
- 238000012986 modification Methods 0.000 description 3
- 238000011160 research Methods 0.000 description 3
- 239000000725 suspension Substances 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical class CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- 208000034486 Multi-organ failure Diseases 0.000 description 2
- 208000010718 Multiple Organ Failure Diseases 0.000 description 2
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 2
- 238000003556 assay Methods 0.000 description 2
- 238000002983 circular dichroism Methods 0.000 description 2
- 201000010099 disease Diseases 0.000 description 2
- 208000037265 diseases, disorders, signs and symptoms Diseases 0.000 description 2
- 230000002708 enhancing effect Effects 0.000 description 2
- 231100000518 lethal Toxicity 0.000 description 2
- 230000001665 lethal effect Effects 0.000 description 2
- 208000029744 multiple organ dysfunction syndrome Diseases 0.000 description 2
- 229910000510 noble metal Inorganic materials 0.000 description 2
- 238000001878 scanning electron micrograph Methods 0.000 description 2
- 229910052710 silicon Inorganic materials 0.000 description 2
- 239000010703 silicon Substances 0.000 description 2
- 230000008685 targeting Effects 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 230000035899 viability Effects 0.000 description 2
- 235000012431 wafers Nutrition 0.000 description 2
- SXRSQZLOMIGNAQ-UHFFFAOYSA-N Glutaraldehyde Chemical compound O=CCCCC=O SXRSQZLOMIGNAQ-UHFFFAOYSA-N 0.000 description 1
- 206010061218 Inflammation Diseases 0.000 description 1
- XUJNEKJLAYXESH-REOHCLBHSA-N L-Cysteine Chemical compound SC[C@H](N)C(O)=O XUJNEKJLAYXESH-REOHCLBHSA-N 0.000 description 1
- COLNVLDHVKWLRT-QMMMGPOBSA-N L-phenylalanine Chemical compound OC(=O)[C@@H](N)CC1=CC=CC=C1 COLNVLDHVKWLRT-QMMMGPOBSA-N 0.000 description 1
- 206010028980 Neoplasm Diseases 0.000 description 1
- 238000003917 TEM image Methods 0.000 description 1
- 102100027881 Tumor protein 63 Human genes 0.000 description 1
- 239000003242 anti bacterial agent Substances 0.000 description 1
- 229940088710 antibiotic agent Drugs 0.000 description 1
- 239000003139 biocide Substances 0.000 description 1
- 230000008033 biological extinction Effects 0.000 description 1
- 238000012984 biological imaging Methods 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 210000001175 cerebrospinal fluid Anatomy 0.000 description 1
- 238000012512 characterization method Methods 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- XUJNEKJLAYXESH-UHFFFAOYSA-N cysteine Natural products SCC(N)C(O)=O XUJNEKJLAYXESH-UHFFFAOYSA-N 0.000 description 1
- 235000018417 cysteine Nutrition 0.000 description 1
- 238000003745 diagnosis Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000012470 diluted sample Substances 0.000 description 1
- 229940079593 drug Drugs 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 230000005684 electric field Effects 0.000 description 1
- 238000002073 fluorescence micrograph Methods 0.000 description 1
- 244000053095 fungal pathogen Species 0.000 description 1
- 230000005182 global health Effects 0.000 description 1
- 210000003709 heart valve Anatomy 0.000 description 1
- 230000005745 host immune response Effects 0.000 description 1
- 238000003384 imaging method Methods 0.000 description 1
- 239000007943 implant Substances 0.000 description 1
- 238000011534 incubation Methods 0.000 description 1
- 230000004054 inflammatory process Effects 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 239000002159 nanocrystal Substances 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 230000004768 organ dysfunction Effects 0.000 description 1
- COLNVLDHVKWLRT-UHFFFAOYSA-N phenylalanine Natural products OC(=O)C(N)CC1=CC=CC=C1 COLNVLDHVKWLRT-UHFFFAOYSA-N 0.000 description 1
- 230000010399 physical interaction Effects 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 208000013223 septicemia Diseases 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 239000004332 silver Substances 0.000 description 1
- 238000004544 sputter deposition Methods 0.000 description 1
- 238000010186 staining Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 230000004083 survival effect Effects 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 230000009885 systemic effect Effects 0.000 description 1
- 230000008718 systemic inflammatory response Effects 0.000 description 1
- 230000003685 thermal hair damage Effects 0.000 description 1
- 210000001519 tissue Anatomy 0.000 description 1
- 230000000451 tissue damage Effects 0.000 description 1
- 231100000827 tissue damage Toxicity 0.000 description 1
- 239000006150 trypticase soy agar Substances 0.000 description 1
- 230000002792 vascular Effects 0.000 description 1
- 244000052613 viral pathogen Species 0.000 description 1
- 230000003612 virological effect Effects 0.000 description 1
Images
Landscapes
- Agricultural Chemicals And Associated Chemicals (AREA)
Abstract
The invention belongs to the technical field of material chemistry, and particularly discloses a chiral gold nano antibacterial material and a preparation method thereof. According to the invention, the gold nanometer bipyramid is used as a seed, and different chiral gold nanometer materials with sea cucumber-like appearances are obtained through the added chiral ligand. The transmission electron microscope proves that the prepared nano structure has good dispersibility and uniformity, the synthesized sea cucumber-like chiral gold nano material has a stable structure, and the prepared sample does not change after being placed at normal temperature for a long time. Meanwhile, the product obtained by the method has excellent chiral property, good photo-thermal effect and obvious sterilization effect.
Description
Technical Field
The invention belongs to the field of material chemistry, and particularly relates to a chiral gold nano antibacterial material and a preparation method thereof.
Background
The noble metal nano material (gold and silver) attracts a lot of researches due to the characteristics of high specific surface, controllable appearance, many surface binding sites and the like. In recent years, the research on the controllable preparation of the size, shape and composition of metal nanoparticles has become a hot spot, and meanwhile, the research on the surface plasma performance of the metal nanoparticles also provides more routes and wide applications, including photoelectrocatalysis, nano biosensors, tumor biological imaging and medical diagnosis and treatment. The wet chemical synthesis method is widely applied to the preparation of noble metal nano particles due to low cost and large scale.
In addition to gold nanorods, gold nanopyramids are another elongated gold nanocrystal with tunable longitudinal plasmon resonance wavelength (LSPR). The gold nanometer bipyramid consists of two pentagonal prisms with the bottoms connected together, has two sharp vertexes, and is more stable than a gold rod. Compared with the gold nanorods, the gold nanopyramids have sharper top ends and narrower appearance and size distribution, so the extinction cross section and the local electric field of the gold nanopyramids are enhanced more than those of the gold nanorods.
Sepsis (sepsis) is a life-threatening disease that results from a dysregulated host immune response to infection, resulting in tissue damage and organ dysfunction with a high mortality rate. The etiology is mainly related to bacterial (gram-negative and gram-positive), viral and fungal pathogens. Staphylococcus epidermidis is the most common organism in foreign implant-related infections, such as prosthetic joints, central venous catheters, cerebrospinal fluid shunts, intracardiac devices, prosthetic heart valves, and vascular grafts. In addition, drug-resistant bacteria have become a serious global health problem due to the widespread overuse of antibiotics and the formation of biofilms. Due to the adjustable physicochemical characteristics (such as shape, particle size, surface charge, composition and the like) and the characteristics of easy surface modification and the like, the nano material has huge potential in the aspect of treating diseases such as septicemia and implantable bacterial infection.
Disclosure of Invention
The invention designs a chiral gold nano material with adjustable plasma resonance peak and sea cucumber-like appearance on the basis of a gold nano bipyramid for resisting bacteria and biomembrane infection, and provides a promising nano tool for resisting lethal bacterial infection, adjusting systemic inflammatory response, preventing multiple organ failure and the like and improving the treatment effect of sepsis. The preparation method of the chiral gold nano antibacterial material comprises the following specific steps:
(1) to HAuCl4Adding a citric acid solution into the solution, uniformly mixing, adding a reducing agent, and reacting to obtain a gold seed solution;
(2) carrying out heat treatment on the gold seed solution;
(3) adding the gold seed solution after heat treatment into a gold nano bipyramid solution to obtain a gold nano bipyramid solution, wherein the gold nano bipyramid solution is a mixed solution of CTAB, silver nitrate, hydrochloric acid and ascorbic acid;
(4) adding a chiral dipeptide aqueous solution and the gold nanometer bipyramid solution into a growth solution to react to prepare the chiral gold nanometer antibacterial material, wherein the growth solution is prepared from CTAB and HAuCl4The mixed solution is prepared by adding ascorbic acid solution.
Preferably, in the step (1), the reducing agent is NaBH4And/or KBH4。
Preferably, the concentration of the gold seed solution is 0.2-0.3 mM.
Preferably, in the step (2), the heat treatment is performed under the condition of stirring at 70-90 ℃ for 60-120 min.
Preferably, in the step (3), the molar ratio of CTAB, silver nitrate, hydrochloric acid and Ascorbic Acid (AA) in the water growth solution is 1000:1-5:1-5: 10-20.
Specifically, the aqueous growth solution may be prepared by mixing 10mL of CTAB solution (100mM), 0.1-0.5mL of silver nitrate aqueous solution (10mM), 1-5mL of hydrochloric acid (1M), and 0.1-0.2mL of AA solution (100 mM).
Preferably, the chiral dipeptide is a dipeptide obtained by condensing cysteine and phenylalanine, and is L-CF, D-CF or DL-CF.
Preferably, in the step (4), Au in the gold nano-bipyramid solution3+、CTAB、HAuCl4Ascorbic acid and chiral dipeptide in a molar ratio of 1-25: 5-100: 1.5-4.5: 7.5-12.5: 0.04-0.12. CTAB solution with concentration of 5-100mM, HAuCl4The concentration of the aqueous solution is 5-15mM, the concentration of the ascorbic acid solution is 75-125mM, and the concentration of the L/D-CF solution is 0.5-1.5 mM; CTAB solution, HAuCl4The volume ratio of the aqueous solution, the ascorbic acid solution and the L/D-CF aqueous solution is 1: 0.3: 0.1: 0.08.
preferably, in the step (4), the reaction condition is that the reaction is carried out for 1.5 to 2.5 hours at the temperature of between 25 and 35 ℃.
The invention provides a chiral gold nano antibacterial material prepared by the preparation method.
Further, the particle size range of the chiral gold nano antibacterial material is 80-150 nm.
Compared with the prior art, the technical scheme of the invention has the following advantages:
the product has good photothermal effect and chiral property, and has targeting effect on bacteria. The biological membrane-killing agent has good performance in killing planktonic bacteria and removing biological membranes, and simultaneously solves the potential thermal damage problem of normal tissues caused by the fact that the traditional treatment means does not target bacteria. The invention constructs a chiral dipeptide functionalized gold nanometer bipyramid material which is used for enhancing PTT based on chemical and physical interaction with bacteria and has obvious bactericidal effect.
Drawings
FIG. 1 is a flow chart of the preparation method of the chiral gold nano antibacterial material of the invention.
FIG. 2 is a transmission electron micrograph and SEM photograph of the chiral gold nano antibacterial material prepared by the invention.
FIG. 3 is a Circular Dichroism (CD) diagram of the chiral gold nano antibacterial material prepared by the invention.
FIG. 4 is an ultraviolet image of the chiral gold nano antibacterial material prepared by the present invention.
FIG. 5 is a graph showing the temperature change of Staphylococcus epidermidis solutions treated by different methods.
FIG. 6 is a graph showing the bacterial viability of Staphylococcus epidermidis after treatment by different methods.
FIG. 7 is a bacterial colony of Staphylococcus epidermidis after treatment by different methods.
FIG. 8 is a live/dead fluorescence image of bacteria treated by different methods (live/dead bacteria were stained with green/red fluorescence, respectively).
FIG. 9 is an SEM image of Staphylococcus epidermidis after treatment by different methods.
Detailed Description
The present invention is further described below in conjunction with the following figures and specific examples so that those skilled in the art may better understand the present invention and practice it, but the examples are not intended to limit the present invention.
Example 1
0.025mL of 100mM HAuCl was taken4Adding 3mL of water into the solution, and mixing to obtain a solution A; to solution A was added 5mL of 100mM CTAC (cetyltrimethylammonium chloride) and 1mL of 50mM citric acid solution, and after stirring well, 0.625mL of 100mM NaBH was added immediately4The solution was stirred for 3min to obtain solution B. The solution B was stirred in an oil bath at 80 ℃ for 90min to give a 0.25mM gold seed solution, which was concentrated to give a 100mM gold seed solution C. Meanwhile, a water growth solution containing 10mL of 100mM hexadecyltrimethylammonium bromide aqueous solution (CTAB), 0.2mL of 10mM silver nitrate, 2mL of 1M hydrochloric acid, 0.15mL of 100mM ascorbic acid was prepared, 100. mu.L of a gold seed solution C was added thereto, stored at 30 ℃ for 2 hours, centrifuged, and the precipitate thereof was dissolved in 1mL of 0.1mol/L CTAB solution to obtain a gold nanopyramid solution D.
To 20mL of the aqueous solution were added 1mL of 100mM CTAB solution and 0.3mL of 10mM HAuCl4And stirring the solution, adding 0.1mL of 100mM ascorbic acid solution to obtain a growth solution A, adding 0.08mL of 1mM chiral dipeptide (DL-CF) solution into the growth solution A, adding 0.4mL of gold nano bipyramid solution D, and standing at 30 ℃ for 2h to obtain the chiral gold nano antibacterial material DL-GBPs with the sea cucumber-like morphology.
Example 2
0.025mL of 100mM HAuCl was taken4Adding 3mL of water into the solution, and mixing to obtain a solution A; to solution A was added 5mL of 100mM CTAC and 1mL of 50mM citric acid solution, and after stirring well, 0.625mL of 100mM NaBH was added immediately4The solution was stirred for 3min to obtain solution B. The solution B was stirred in an oil bath at 80 ℃ for 90min to give a 0.25mM gold seed solution, which was concentrated to give a 100mM gold seed solution C. Simultaneously preparing water growth solution containing 10mL of 100mM CTAB, 0.2mL of 10mM silver nitrate, 2mL of 1M hydrochloric acid and 0.15mL of 100mM ascorbic acid, adding the gold seed solution C, standing and storing at 30 ℃ for 2h, centrifuging, dissolving the precipitate in 1mL of 0.1mol/L CTAB solution to obtain the gold nano bipyramidAnd (D) solution.
To 20mL of the aqueous solution were added 1mL of 95mM CTAB solution and 0.3mL of 12mM HAuCl4And stirring the solution, adding 0.1mL of 110mM ascorbic acid solution to obtain a growth solution A, adding 0.08mL of 1.0mM chiral dipeptide (L-CF) solution into the growth solution A, adding 0.4mL of gold nano bipyramid solution D, and standing at 30 ℃ for 2h to obtain the chiral gold nano antibacterial material L-GBPs with the sea cucumber-like morphology.
Example 3
0.025mL of 100mM HAuCl was taken4Adding 3mL of water into the solution, and mixing to obtain a solution A; to solution A was added 5mL of 100mM CTAC and 1mL of 50mM citric acid solution, and after stirring well, 0.625mL of 100mM NaBH was added immediately4The solution was stirred for 3min to obtain solution B. The solution B was stirred in an oil bath at 80 ℃ for 90min to give a 0.25mM gold seed solution, which was concentrated to give a 100mM gold seed solution C. Meanwhile, preparing a water growth solution containing 10mL of 100mM CTAB, 0.2mL of 10mM silver nitrate, 2mL of 1M hydrochloric acid and 0.15mL of 100mM ascorbic acid, adding the gold seed solution C into the water growth solution, standing and storing the mixture for 2 hours at 30 ℃, centrifuging the mixture, and dissolving the precipitate in 1mL of 0.1mol/L CTAB solution to obtain a gold nano bipyramid solution D.
To 20mL of the aqueous solution were added 1mL of 100mM CTAB solution and 0.3mL of 10mM HAuCl4And stirring the solution, adding 0.1mL of 100mM ascorbic acid solution to obtain a growth solution A, adding 0.08mL of 1.0mM chiral dipeptide (D-CF) solution into the growth solution A, adding 0.4mL of gold nano-bipyramid solution D, and standing at 30 ℃ for 2h to obtain the chiral gold nano-materials D-GBPs with the sea cucumber-like morphology.
Example 4
0.025mL of 100mM HAuCl was taken4Adding 4mL of water into the solution, and mixing to obtain a solution A; to solution A was added 5mL of 100mM CTAC and 1mL of 50mM citric acid solution to solution A, and after stirring well, 0.625mL of 100mM NaBH was added immediately4The solution was stirred for 4min to obtain solution B. The solution B was stirred in a 70 ℃ oil bath for 120min to give a 0.25mM gold seed solution, which was concentrated to give a 100mM gold seed solution C. While preparing a water growth solution containing 10mL of 100mM CTAB, 0.2mL of 10mM silver nitrate, 1mL of 1M hydrochloric acid and 0.15mL of 100mM ascorbic acid, gold seeds were added theretoAnd standing and storing the solution C at 30 ℃ for 2h, centrifuging at 6000rpm for 10min, and dissolving the precipitate in 1mL of 0.1mol/L CTAB solution to obtain a gold nano bipyramid solution D.
To 20mL of the aqueous solution were added 1mL of 100mM CTAB solution and 0.3mL of 10mM HAuCl4And stirring the solution, adding 0.1mL of 100mM ascorbic acid solution to obtain a growth solution A, adding 0.08mL of 1.0mM chiral dipeptide (D-CF) solution into the growth solution A, adding 0.4mL of gold nano-bipyramid solution D, and standing at 30 ℃ for 2h to obtain the chiral gold nano-materials D-GBPs with the sea cucumber-like morphology.
Example 5
0.025mL of 100mM HAuCl was taken4Adding 4mL of water into the solution, and mixing to obtain a solution A; 5mL of 100mM CTAC and 1mL of 50mM citric acid solution were added to solution A, and after stirring well, 0.625mL of 100mM NaBH was added immediately4The solution was stirred for 4min to obtain solution B. The solution B was stirred in an oil bath at 90 ℃ for 60min to give a 0.25mM gold seed solution, which was concentrated to give a 100mM gold seed solution C. Meanwhile, preparing a water growth solution containing 10mL of 100mM CTAB, 0.2mL of 10mM silver nitrate, 1mL of 1M hydrochloric acid and 0.15mL of 100mM ascorbic acid, adding the gold seed solution C into the water growth solution, standing and storing the mixture for 2 hours at 30 ℃, centrifuging the mixture, and dissolving the precipitate in 1mL of 0.1mol/L CTAB solution to obtain a gold nano bipyramid solution D.
To 20mL of the aqueous solution were added 1mL of 100mM CTAB solution and 0.3mL of 10mM HAuCl4And stirring the solution, adding 0.1mL of 100mM ascorbic acid solution to obtain a growth solution A, adding 0.08mL of 1.0mM chiral dipeptide (D-CF) solution into the growth solution A, adding 0.4mL of gold nano-bipyramid solution D, and standing at 30 ℃ for 2h to obtain the chiral gold nano-materials D-GBPs with the sea cucumber-like morphology.
Antibacterial tests were performed on PBS, PEG-Au NBP, examples 1,2 and 3, and 100. mu.L of bacterial suspension (2X 10)4(Staphylococcus epidermidis in CFU)/mL (TSB) and 100. mu.L of 0.01M PBS, PEG-Au NBPs, DL-GBPs, D-GBPs and L-GBPs were added to wells of a 96-well plate, respectively. The mixture was vortexed for 3min, then placed in an incubator for 3h, and then irradiated with 808nm laser for 5min (0.8W/cm)2). After irradiation, the mixture was incubated at 37 ℃ for a further 12h. Finally, the value of optical density was measured at 600nm using a microplate reader. The results are shown in FIG. 6, using bacterial suspensions cultured on unirradiated samples as controls.
In a standard plate count assay, bacterial suspensions were serially diluted with 0.01M sterile PBS and 100. mu.L of each diluted sample was plated on tryptic soy agar plates. After incubation at 37 ℃ for 12h, colonies formed on the surface of the plate were counted to evaluate the bacterial concentration. The results are shown in FIG. 7.
LIVE/DEAD staining assays of bacteria were performed on PBS, PEG-Au NBP and examples 1,2,3, and treated bacteria were stained with LIVE/DEAD BacLight bacterial viability kit and viewed by Axio vert. a1 fluorescence microscope imaging system. The results are shown in FIG. 8.
SEM images were taken to observe the morphology of PBS, PEG-AuNBP, examples 1,2,3 in irradiated and non-irradiated bacteria.
The differently treated staphylococcus epidermidis solutions were dropped onto silicon wafers, then fixed with 2% glutaraldehyde at room temperature for 3h, then dehydrated in a series of ethanol solutions (50%, 70%, 90%, 95% and 100%) gradient for 10min each step.
The silicon wafers were dried under nitrogen flow, plated with ultra-thin gold coatings by sputtering, and imaged at 3.0kV using hitachi Su8010 instrument. The results are shown in FIG. 9.
Through a series of material performance characterization comparison, the invention successfully prepares the sea cucumber-shaped chiral gold nano antibacterial material. Tests on photo-thermal effect, survival performance of bacteria and the like show that the sea cucumber-like chiral gold nano material can be sterilized by targeting bacteria and enhancing PTT effect, and the sterilizing effect is obvious.
Therefore, the sea cucumber-like chiral gold nano antibacterial material prepared by the invention provides a promising nano tool for resisting lethal bacterial infection, regulating systemic inflammatory reaction, preventing multiple organ failure and the like and improving the treatment effect of sepsis.
It should be understood that the above examples are only for clarity of illustration and are not intended to limit the embodiments. Other variations and modifications will be apparent to persons skilled in the art in light of the above description. And are neither required nor exhaustive of all embodiments. And obvious variations or modifications of the invention may be made without departing from the spirit or scope of the invention.
Claims (10)
1. A preparation method of a chiral gold nano antibacterial material is characterized by comprising the following steps:
(1) to HAuCl4Adding a citric acid solution into the solution, uniformly mixing, adding a reducing agent, and reacting to obtain a gold seed solution;
(2) carrying out heat treatment on the gold seed solution;
(3) adding the gold seed solution after heat treatment into a gold nano bipyramid solution to obtain a gold nano bipyramid solution, wherein the gold nano bipyramid solution is a mixed solution of CTAB, silver nitrate, hydrochloric acid and ascorbic acid;
(4) adding a chiral dipeptide aqueous solution and the gold nanometer bipyramid solution into a growth solution to react to prepare the chiral gold nanometer antibacterial material, wherein the growth solution is prepared from CTAB and HAuCl4Adding ascorbic acid solution into the mixed solution to obtain the final product.
2. The method for preparing chiral gold nano antibacterial material according to claim 1, wherein in the step (1), the reducing agent is NaBH4And/or KBH4。
3. The method for preparing the chiral gold nano antibacterial material according to claim 1, wherein the concentration of the gold seed solution is 0.2-0.3 mM.
4. The method for preparing the chiral gold nano antibacterial material according to claim 1, wherein in the step (2), the heat treatment condition is stirring at 70-90 ℃ for 60-120 min.
5. The method for preparing chiral gold nano antibacterial material according to claim 1, characterized in that in the step (3), the molar ratio of CTAB, silver nitrate, hydrochloric acid and ascorbic acid in the water growth solution is 1000:1-5:1-5: 10-20.
6. The method for preparing chiral gold nano-antibacterial material according to claim 1, wherein the chiral dipeptide is L-CF, D-CF or DL-CF.
7. The method for preparing chiral gold nano antibacterial material according to claim 1, wherein in the step (4), Au is contained in the gold nano bipyramid solution3+、CTAB、HAuCl4Ascorbic acid and chiral dipeptide in a molar ratio of 1-25: 5-100: 1.5-4.5: 7.5-12.5: 0.04-0.12.
8. The method for preparing the chiral gold nano antibacterial material according to claim 1, wherein in the step (4), the reaction is carried out at 25-35 ℃ for 1.5-2.5 h.
9. A chiral gold nano antibacterial material prepared by the preparation method of any one of claims 1-8.
10. The chiral gold nano-antibacterial material according to claim 9, wherein the particle size of the chiral gold nano-antibacterial material is in the range of 80-150 nm.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202111633546.7A CN114309636B (en) | 2021-12-28 | 2021-12-28 | Chiral gold nano antibacterial material and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202111633546.7A CN114309636B (en) | 2021-12-28 | 2021-12-28 | Chiral gold nano antibacterial material and preparation method thereof |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN114309636A true CN114309636A (en) | 2022-04-12 |
| CN114309636B CN114309636B (en) | 2024-01-19 |
Family
ID=81014733
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202111633546.7A Active CN114309636B (en) | 2021-12-28 | 2021-12-28 | Chiral gold nano antibacterial material and preparation method thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN114309636B (en) |
Citations (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103240420A (en) * | 2013-05-24 | 2013-08-14 | 苏州大学 | Purification method for gold nano-particles with double-cone structures |
| CN105834451A (en) * | 2016-05-25 | 2016-08-10 | 东华大学 | Preparation method for gold nanoparticle bipyramids |
| US20180312636A1 (en) * | 2017-04-28 | 2018-11-01 | Lg Display Co., Ltd. | Metal Nanostructure and Method for Manufacturing Thereof |
| CN111112596A (en) * | 2018-11-01 | 2020-05-08 | 国家纳米科学中心 | Chiral noble metal nano-particles and preparation method and application thereof |
| CN111230136A (en) * | 2020-03-30 | 2020-06-05 | 江南大学 | Synthesis method of asymmetric chiral gold rod @ copper @ gold nanorod |
| CN111494618A (en) * | 2020-04-23 | 2020-08-07 | 江南大学 | Preparation method and application of chiral nano material adjuvant |
| KR20210041504A (en) * | 2019-10-04 | 2021-04-15 | 서울대학교산학협력단 | Method of fabricating 3-dimensional chiral metal nanostructure and 3-dimensional chiral metal nanostructure fabricated therefrom |
| CN112828283A (en) * | 2020-12-31 | 2021-05-25 | 纳米籽有限公司 | High-purity gold nanoparticles, selectively-coated gold nanoparticles and preparation method thereof |
| CN112889840A (en) * | 2021-01-15 | 2021-06-04 | 南京农业大学 | Chiral cysteine nano self-assembly antibacterial material and preparation method and application thereof |
-
2021
- 2021-12-28 CN CN202111633546.7A patent/CN114309636B/en active Active
Patent Citations (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103240420A (en) * | 2013-05-24 | 2013-08-14 | 苏州大学 | Purification method for gold nano-particles with double-cone structures |
| CN105834451A (en) * | 2016-05-25 | 2016-08-10 | 东华大学 | Preparation method for gold nanoparticle bipyramids |
| US20180312636A1 (en) * | 2017-04-28 | 2018-11-01 | Lg Display Co., Ltd. | Metal Nanostructure and Method for Manufacturing Thereof |
| CN110573280A (en) * | 2017-04-28 | 2019-12-13 | 乐金显示有限公司 | Metal nanostructure and method of making same |
| CN111112596A (en) * | 2018-11-01 | 2020-05-08 | 国家纳米科学中心 | Chiral noble metal nano-particles and preparation method and application thereof |
| KR20210041504A (en) * | 2019-10-04 | 2021-04-15 | 서울대학교산학협력단 | Method of fabricating 3-dimensional chiral metal nanostructure and 3-dimensional chiral metal nanostructure fabricated therefrom |
| CN111230136A (en) * | 2020-03-30 | 2020-06-05 | 江南大学 | Synthesis method of asymmetric chiral gold rod @ copper @ gold nanorod |
| CN111494618A (en) * | 2020-04-23 | 2020-08-07 | 江南大学 | Preparation method and application of chiral nano material adjuvant |
| CN112828283A (en) * | 2020-12-31 | 2021-05-25 | 纳米籽有限公司 | High-purity gold nanoparticles, selectively-coated gold nanoparticles and preparation method thereof |
| CN112889840A (en) * | 2021-01-15 | 2021-06-04 | 南京农业大学 | Chiral cysteine nano self-assembly antibacterial material and preparation method and application thereof |
Non-Patent Citations (1)
| Title |
|---|
| 许富刚;谢施;任春锦;冯亚楠;曹仁涛;: "一种通用的合成多刺状的银@金和银@金@银纳米结构的方法用于提高表面增强拉曼的活性", 吉林师范大学学报(自然科学版), vol. 38, no. 01, pages 19 - 26 * |
Also Published As
| Publication number | Publication date |
|---|---|
| CN114309636B (en) | 2024-01-19 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| Zhang et al. | Near-infrared-triggered antibacterial and antifungal photodynamic therapy based on lanthanide-doped upconversion nanoparticles | |
| CN114306382B (en) | Copper-based nanoenzyme as well as preparation method and application thereof | |
| CN110028553B (en) | Preparation method and application of antibacterial nanoprobe Au-PEG-AMP-Ce6 | |
| Ranganath et al. | Screening of Lactobacillus spp, for mediating the biosynthesis of silver nanoparticles from silver nitrate | |
| CN107971481A (en) | Gold nanoclusters with antibacterial activity and its preparation method and application | |
| CN113016823B (en) | Preparation method of photo-thermal antibacterial near-infrared bimetallic nanoparticles | |
| Wang et al. | Construction of perfluorohexane/IR780@ liposome coating on Ti for rapid bacteria killing under permeable near infrared light | |
| JP2012526777A (en) | Biocide Nanostructured Composition and Method for Obtaining Nanostructured Biocide Composition | |
| Farajzadeh et al. | The design and synthesis of metallophthalocyanine–gold nanoparticle hybrids as biological agents | |
| Shao et al. | Light activation of gold nanorods but not gold nanospheres enhance antibacterial effect through photodynamic and photothermal mechanisms | |
| Kalia et al. | Antimycotic activity of biogenically synthesised metal and metal oxide nanoparticles against plant pathogenic fungus Fusarium moniliforme (F. fujikuroi) | |
| Chakraborty et al. | Silver nanoparticle synthesis and their potency against multidrug-resistant bacteria: a green approach from tissue-cultured Coleus forskohlii | |
| CN109111178A (en) | Ceramic material with active slow release effect, method for its manufacture and system comprising such ceramic material | |
| CN114734032A (en) | Method for preparing nano-silver based on kapok extract | |
| CN114469893A (en) | Quaternary ammonium salinized silicon dioxide nano-particles, preparation method and application | |
| Faiq et al. | Inhibitory effects of biosynthesized copper nanoparticles on biofilm formation of Proteus mirabilis | |
| CN114309636B (en) | Chiral gold nano antibacterial material and preparation method thereof | |
| Rashid et al. | Characterization and antimicrobial efficiency of silver nanoparticles based reduction method | |
| Kanchana et al. | Plant mediated synthesis of silver nanoparticles with diverse applications | |
| RU2379042C1 (en) | Biologically active preparation | |
| CN108721248A (en) | A kind of preparation method, product and the application of pH response type nanos silver assembly | |
| Kumar et al. | Green synthesis and biochemical characterization of silver nanoparticles by using Euphorbia umbellata leaf extract and analysis of antimicrobial activity against plant pathogens | |
| Usha et al. | A Study on Silver Nano Particle Production from Aristolochia Bracteata and Its Antimicrobial Activity | |
| KR101730604B1 (en) | core-shell nanocomposites showing antibacterial, method for manufacturing thereof and uses thereof | |
| Bozer et al. | Green Synthesized Zinc Oxide Nanoparticles with Salvadora persica L. Root Extract and Their Antagonistic Activity Against Oral and Health-Threatening Pathogens |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |