CN109735330B - Iron ion doped carbon dot, preparation method and application thereof - Google Patents
Iron ion doped carbon dot, preparation method and application thereof Download PDFInfo
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Abstract
The invention belongs to the technical field of nano medicine, and particularly relates to iron ion doped carbon dots, a preparation method and application thereof. The invention discloses a preparation method of iron ion doped carbon dots, which takes citric acid, urea, cobalt nitrate, EDTA and ferric chloride as main raw materials, and has the advantages of simple and environment-friendly process, cheap and easily-obtained raw materials, high yield, low cost and the like.
Description
Technical Field
The invention belongs to the technical field of nano-medicine, and particularly relates to iron ion doped carbon dots, a preparation method and application thereof.
Background
The nano material has the characteristics of broad-spectrum sterilization property, excellent antibacterial performance, difficult generation of drug resistance of pathogenic microorganisms to the nano material and the like, and is widely applied to the antibacterial field. The quantum dots are special nanoparticles with the size of 1-100nm, at present, a subject group has researches on applying Cd quantum dots to the aspect of antibiosis, a possible antibacterial mechanism is that the Cd quantum dots change the permeability of cell membranes so as to promote bacterial death, but the biocompatibility of the Cd quantum dots is poor. The carbon dot is a novel carbon-based zero-dimensional material, and has good optical performance, photochemical stability, water solubility, biocompatibility and low cytotoxicity. However, the application of the carbon dots in the aspect of antibiosis is only rarely reported in the literature.
Disclosure of Invention
The invention aims to provide a preparation method of iron ion doped carbon dots, which has the advantages of simple and environment-friendly process, cheap and easily-obtained raw materials, high yield, low cost and the like.
The invention also aims to provide the functionalized iron ion doped carbon dot which has the characteristics of good bacteriostatic action, good water solubility, low cytotoxicity and the like.
Still another object of the present invention is to provide the use of the iron ion-doped carbon dots for preparing an antibacterial agent.
In order to achieve the purpose, the technical scheme of the invention is as follows:
the invention provides a preparation method of iron ion doped carbon dots, which comprises the following steps:
step 1: dissolving citric acid, urea, cobalt nitrate and EDTA in N, N-dimethylformamide, and preparing carbon dots by adopting a hydrothermal method;
step 2: and (3) adding the carbon dots obtained in the step (1) into an ultrapure water solution of ferric chloride, heating for reaction, and drying to obtain iron ion doped carbon dots.
Preferably, in the step 1, the feeding ratio of citric acid, urea, cobalt nitrate and EDTA is 1.
Preferably, in the step 1, the reaction temperature is 120 ℃ and the reaction time is 8h.
Preferably, in the step 2, the weight ratio of the ferric chloride to the carbon dots in the step 1 is 0 to 16.7/100.
Preferably, in the step 2, the reaction temperature is 95 ℃ and the reaction time is 20 minutes.
Preferably, in the step 2, the drying temperature is 100 ℃.
The iron ion doped carbon dots prepared by any one of the methods are also within the protection scope of the invention.
The invention also provides application of the iron ion doped carbon dots prepared by any one of the methods in preparation of an antibacterial agent, wherein the iron ion doped carbon dots are independently used as effective components, or the iron ion doped carbon dots and the antibacterial agent are combined to be used as effective components, and the resisted or inhibited microbial bacteria comprise bacteria and/or fungi, such as staphylococcus aureus, escherichia coli and other bacteria.
The invention achieves the following beneficial effects:
(1) The preparation method of the iron ion doped carbon dots has the advantages of simple and environment-friendly process, cheap and easily-obtained raw materials, high yield, low cost and the like.
(2) The iron ion doped carbon dots have good dispersion performance, but the particle size is increased along with the increase of the concentration of the iron ions.
(3) The iron ion doped carbon dot has good inhibition effect on escherichia coli and staphylococcus aureus, and the inhibition effect is enhanced along with the increase of the concentration of the iron ions.
(4) The iron ion doped carbon dots prepared by the invention have the characteristics of low hemolytic toxicity, good biocompatibility, low cytotoxicity and the like, and can become a good antibacterial agent capable of being administered systemically.
Drawings
FIG. 1 is a projection electron microscope (TEM) image of a carbon dot not doped with iron ions;
fig. 2 is a projection electron microscope (TEM) image of iron ion doped carbon dots at ferric chloride/carbon dot = 5.3/100;
fig. 3 is a projection electron microscope (TEM) image of iron ion doped carbon dots at ferric chloride/carbon dot = 10.7/100;
fig. 4 is a projection electron microscope (TEM) image of iron ion doped carbon dots at iron chloride/carbon dot = 16.7/100;
FIG. 5 is a graph of an infrared absorption spectrum of iron ion doped carbon dots;
FIG. 6 is a graph showing the ultraviolet absorption spectrum of carbon dots doped with iron ions
FIG. 7 is a graph showing the inhibitory effect of iron ion-doped carbon dots on Escherichia coli;
FIG. 8 is a graph showing the inhibitory effect of iron ion-doped carbon dots on Staphylococcus aureus;
FIG. 9 shows the MTT test results of the iron ion-doped carbon dots on A549 cells;
FIG. 10 is a graph of iron ion-doped carbon dot hemolysis;
description of the drawings: in the drawing, 1 indicates the experimental result of the carbon spot not doped with ferric chloride, 2 indicates the experimental result of the carbon spot doped with ferric ions when the ferric chloride/carbon spot =5.3/100, 3 indicates the experimental result of the carbon spot doped with ferric ions when the ferric chloride/carbon spot =10.7/100, and 4 indicates the experimental result of the carbon spot doped with ferric ions when the ferric chloride/carbon spot = 16.7/100.
Detailed Description
The present invention will now be described more fully hereinafter with reference to the accompanying specific embodiments, in which some, but not all embodiments of the invention are shown. All other embodiments that can be derived from the embodiments of the present invention by a person skilled in the art are within the scope of the present invention.
Example 1 preparation of iron ion-doped carbon dots (iron chloride/carbon dots = 5.3/100)
Step 1: adding 6.0g of citric acid, 12.0g of urea, 12.0g of cobalt nitrate and 12.0g of EDTA into a 50ml beaker, adding 40ml of N, N-dimethylformamide, stirring and dissolving by using a glass rod, transferring the mixture into a 50ml reaction kettle, screwing a kettle cover, placing the kettle cover into a forced air drying oven, controlling the temperature to be 120 ℃ for reaction for 8 hours, naturally cooling a reaction system to room temperature after the reaction is finished, carrying out centrifugal separation, discarding supernatant, centrifugally washing the centrifugal solid for 5 times (10000 rpm/min,5 min) by using 2M sodium hydroxide ethanol solution, controlling the temperature of the centrifugally obtained solid for drying for 4 hours at 60 ℃ to obtain 12.6g of solid powder, wherein the carbon point yield is 43.4%, and the carbon point hydration kinetic particle size is 5.7 +/-1.1 nm.
Step 2: weighing 3.2mg of ferric chloride solid, adding into a reaction bottle, adding 10ml of ultrapure water for dissolving and clarifying, adding 60.0mg of carbon point in the step 1, controlling the temperature to be 95 ℃, reacting for 20min, pouring into a culture dish, putting into an oven, controlling the temperature to be 100 ℃, and drying to obtain 50.0mg of black solid, wherein the yield is 79.1%, and the particle size is 8.9 +/-2.5 nm.
Example 2 preparation of iron ion doped carbon dots (iron chloride/carbon dots = 10.7/100)
Step 1: carbon dots were prepared according to the method described in example 1, step 1.
Step 2: weighing 6.4mg of ferric chloride solid, adding into a reaction bottle, adding 10ml of ultrapure water for dissolving and clarifying, adding 60.0mg of carbon point in the step 1, controlling the temperature to be 95 ℃, reacting for 20min, pouring into a culture dish, putting into an oven, controlling the temperature to be 100 ℃, and drying to obtain 55.0mg of black solid, wherein the yield is 82.8%, and the particle size is 9.5 +/-1.5 nm.
Example 3 preparation of iron ion doped carbon dots (iron chloride/carbon dots = 16.7/100)
Step 1: carbon dots were prepared according to the method described in example 1, step 1.
Step 2: weighing 10.0mg of ferric chloride solid, adding into a reaction bottle, adding 10ml of ultrapure water for dissolving and clarifying, adding 60.0mg of carbon dots in the step 1, controlling the temperature to be 95 ℃, reacting for 20min, pouring into a culture dish, putting into an oven, controlling the temperature to be 100 ℃, and drying to obtain 60.3mg of black solid, wherein the yield is 86.1%, and the particle size is 14.4 +/-3.1 nm.
The experimental result shows that the iron ion-doped carbon dots have a smaller particle size, but the particle size increases with the increase of the iron ion concentration, and when the iron ion doping concentration is increased from 0 to 16.7%, the particle size of the iron ion-doped carbon dots increases from 5.7 + -1.1 nm to 14.4 + -3.1 nm.
Example 4 antimicrobial Activity assay (E.coli)
Taking single escherichia coli colony to shake and culture overnight at 37 ℃ in an LB culture medium, wherein the concentration of the diluted colony is 5 multiplied by 10 5 . 200. Mu.L of the above-mentioned bacterial solution was added to each well of a 96-well plate, 5. Mu.L of iron ion-doped carbon dot dispersions (concentrations of 0.05,0.1,0.2,0.5,1.0,2.0,5.0mg/ml, respectively) of different concentrations were added to each well, and after gentle shaking for 30 seconds, the resulting mixture was incubated overnight at 37 ℃ and the absorbance thereof was measured at 595 nm. The experimental results are as follows:
bacterial survival (%) = (OD) Material –OD Broth only )/(OD H2O+bac –OD Broth only ) X 100% where OD Material The absorbance, OD, of the mixed solution of iron ion doped carbon dot dispersion and bacteria Broth only Absorbance, OD, of the bacterial culture H2O+bac The absorbance of the water and bacteria mixture.
The experimental result shows that the iron ion doped carbon dots have good inhibition effect on escherichia coli, the bacteriostasis effect is enhanced along with the increase of the iron ion concentration, and when the iron ion doped concentration is increased from 0 to 16.7 percent, the half bacteriostasis concentration of the iron ion doped carbon dots on the escherichia coli is reduced from 4.0mg/ml to 0.2mg/ml.
Example 5 antibacterial Activity test (Staphylococcus aureus)
Shaking culturing Staphylococcus aureus single colony in LB culture medium at 37 deg.C overnight, and diluting to 5 × 10 5 . mu.L of the above-mentioned bacterial solution was added to each well of a 96-well plate, and 5. Mu.L of dispersions containing silver and carbon dots (each having a concentration of 0.05,0.1,0.2,0.5,1.0,2.0,5.0 mg/ml) at different concentrations were added to each well, followed by gentle shaking for 30 seconds, incubation at 37 ℃ overnight, and absorbance at 595nm was measured. The experimental results are as follows:
the experimental result shows that the iron ion doped carbon dot has good inhibitory effect on Staphylococcus aureus, the bacteriostatic effect is enhanced along with the increase of the iron ion concentration, and when the iron ion doped concentration is increased from 0 to 16.7%, the half inhibitory concentration of the iron ion doped carbon dot on Escherichia coli is reduced from 5.0mg/ml to 0.6mg/ml.
Example 6 cytotoxicity assay
A549 cells in logarithmic growth phase are prepared into 5.0 × 10 3 Single cell suspension per ml, then seeded in 96 well cell culture plates, adding body per wellThe volume is 100. Mu.L, and then it is placed in CO 2 When the culture is carried out in the incubator until the confluence degree is about 80 percent, removing the original culture medium, adding culture media containing iron ion doped carbon dots with different concentrations (the concentrations are respectively 0,0.05,0.1,0.2,0.5 and 1.0 mg/mL), continuously culturing for 24 hours, absorbing the old culture medium, adding 100 mu L of fresh culture medium, adding 20 mu L of MTT (5 mg/mL) into each hole, placing the fresh culture medium in the incubator for continuously culturing for 4 hours, absorbing and removing supernatant, adding 150 mu L of DMSO into each hole, oscillating the fresh culture medium at a low speed in a microplate reader for three times until purple crystals in the holes are completely dissolved, measuring the OD value of each hole at the 595nm wavelength, and recording experimental data results. And calculating the survival rate of the A549 cell strain under the conditions of different dosing concentrations. The experimental results are as follows:
the experimental results show that the carbon point doped with iron ions has lower toxicity to A549 cells, but the cytotoxicity is enhanced along with the increase of the concentration of the iron ions.
Example 7 hemolytic toxicity test
Killing the rat by dislocation of the neck, picking 5mL of blood from the eyeball, adding 0.5mL of heparin sodium solution for anticoagulation, centrifuging for 10min at 3000r/min, washing with normal saline, centrifuging until the supernatant does not become red, removing the supernatant, taking 0.5mL, and adding 49.5mL of normal saline to obtain the erythrocyte suspension. And preparing dispersions of iron ion doped carbon dots with different concentrations (the concentrations are respectively 0,0.05,0.1,0.2,0.5 and 1.0 mg/mL) for later use. 400 μ L of the erythrocyte suspension was added to 1.5mL of the centrifuge tubes, 5 μ L of the material dispersion was added to each centrifuge tube at different concentrations, and the mixture was incubated at 37 ℃ for 1h and centrifuged at 5000r/min for 10min. 200 μ L of supernatant was added to a new 96-well plate. Each concentration was paralleled by 3 groups, using purified water as a blank and Triton X-100 as a complete hemolysis group. The results of the absorbance test of the 96-well plate at 543nm on an microplate reader are as follows:
calculating the hemolysis by the following formula:
degree of hemolysis (%) = (a) Material -A H2O )/(A Complete hemolysis -A H2O )×100％
Wherein A is Material Adding red blood cells into the iron ion-doped carbon dot dispersion liquid, and then obtaining the absorbance of the supernatant A H2O Absorbance of the supernatant after addition of water to the erythrocytes, A Complete hemolysis 1% of absorbance of supernatant after the incorporation of Triton X-100 into erythrocytes.
The experimental result shows that the iron ion doped carbon dots have reduced hemolytic toxicity, but the hemolytic toxicity is enhanced with the increase of the iron ion concentration, and when the iron ion doped concentration is increased from 0 to 16.7%, the half hemolytic concentration of the iron ion doped carbon dots is far more than 1mg/ml.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, but rather as the intention of all modifications, equivalents, improvements, and equivalents falling within the spirit and scope of the invention.
Claims (4)
1. A preparation method of iron ion doped carbon dots comprises the following steps:
step 1: dissolving citric acid, urea, cobalt nitrate and EDTA in N, N-dimethylformamide, and preparing carbon dots by a hydrothermal method;
step 2: adding the carbon dots obtained in the step 1 into an iron chloride ultrapure water solution, heating for reaction, and drying to obtain iron ion doped carbon dots;
in the step 1, the feeding weight ratio of citric acid, urea, cobalt nitrate and EDTA is 1; in the step 2, the weight ratio of the ferric chloride to the carbon dots in the step 1 is 5.3-16.7/100, the reaction temperature is 95 ℃, and the reaction time is 20 minutes.
2. A pharmaceutical composition comprising the iron ion-doped carbon dots prepared by the method of claim 1.
3. Use of the pharmaceutical composition of claim 2 for the preparation of an antibacterial agent.
4. The use of the pharmaceutical composition of claim 3 in the preparation of an escherichia coli inhibitor or a staphylococcus aureus inhibitor.
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