CN114105121A - Starch carbon quantum dot and preparation method and application thereof - Google Patents
Starch carbon quantum dot and preparation method and application thereof Download PDFInfo
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- 229920002472 Starch Polymers 0.000 title claims abstract description 88
- 239000008107 starch Substances 0.000 title claims abstract description 88
- 235000019698 starch Nutrition 0.000 title claims abstract description 88
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 title claims abstract description 64
- 238000002360 preparation method Methods 0.000 title claims abstract description 20
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 29
- 238000000034 method Methods 0.000 claims abstract description 22
- 238000006243 chemical reaction Methods 0.000 claims abstract description 13
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 11
- 241000894006 Bacteria Species 0.000 claims abstract description 10
- 238000001816 cooling Methods 0.000 claims abstract description 10
- 239000012153 distilled water Substances 0.000 claims abstract description 8
- 238000003756 stirring Methods 0.000 claims abstract description 8
- 239000006228 supernatant Substances 0.000 claims abstract description 8
- -1 polytetrafluoroethylene Polymers 0.000 claims abstract description 7
- 239000000706 filtrate Substances 0.000 claims abstract description 6
- 238000001914 filtration Methods 0.000 claims abstract description 6
- 238000004108 freeze drying Methods 0.000 claims abstract description 6
- 230000002401 inhibitory effect Effects 0.000 claims abstract description 6
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims abstract description 6
- 239000004810 polytetrafluoroethylene Substances 0.000 claims abstract description 6
- 239000002244 precipitate Substances 0.000 claims abstract description 6
- 241000192125 Firmicutes Species 0.000 claims abstract description 5
- 241000186779 Listeria monocytogenes Species 0.000 claims description 12
- 239000012528 membrane Substances 0.000 claims description 6
- 241000588724 Escherichia coli Species 0.000 claims description 5
- 241000589517 Pseudomonas aeruginosa Species 0.000 claims description 5
- 241000191967 Staphylococcus aureus Species 0.000 claims description 5
- 238000005119 centrifugation Methods 0.000 claims description 4
- 239000011148 porous material Substances 0.000 claims description 2
- 230000035484 reaction time Effects 0.000 claims description 2
- 238000009777 vacuum freeze-drying Methods 0.000 claims description 2
- 239000002994 raw material Substances 0.000 abstract description 6
- 235000013305 food Nutrition 0.000 abstract description 4
- 238000004519 manufacturing process Methods 0.000 abstract description 4
- 239000003814 drug Substances 0.000 abstract description 3
- 238000009776 industrial production Methods 0.000 abstract description 2
- 239000000243 solution Substances 0.000 description 18
- 230000003385 bacteriostatic effect Effects 0.000 description 17
- 230000000844 anti-bacterial effect Effects 0.000 description 5
- 230000005540 biological transmission Effects 0.000 description 5
- 239000000463 material Substances 0.000 description 5
- 239000002096 quantum dot Substances 0.000 description 5
- 238000011160 research Methods 0.000 description 5
- 229920001817 Agar Polymers 0.000 description 4
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 4
- 239000008272 agar Substances 0.000 description 4
- 229910052799 carbon Inorganic materials 0.000 description 4
- 238000009792 diffusion process Methods 0.000 description 4
- 239000002086 nanomaterial Substances 0.000 description 4
- 238000010586 diagram Methods 0.000 description 3
- 238000002474 experimental method Methods 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 239000011852 carbon nanoparticle Substances 0.000 description 2
- 238000009826 distribution Methods 0.000 description 2
- 229940079593 drug Drugs 0.000 description 2
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- 230000036541 health Effects 0.000 description 2
- 230000005764 inhibitory process Effects 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 238000005303 weighing Methods 0.000 description 2
- FOIXSVOLVBLSDH-UHFFFAOYSA-N Silver ion Chemical compound [Ag+] FOIXSVOLVBLSDH-UHFFFAOYSA-N 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 230000003013 cytotoxicity Effects 0.000 description 1
- 231100000135 cytotoxicity Toxicity 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 239000007850 fluorescent dye Substances 0.000 description 1
- 238000002173 high-resolution transmission electron microscopy Methods 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 125000004435 hydrogen atom Chemical class [H]* 0.000 description 1
- 238000002347 injection Methods 0.000 description 1
- 239000007924 injection Substances 0.000 description 1
- 244000005700 microbiome Species 0.000 description 1
- 238000000593 microemulsion method Methods 0.000 description 1
- 238000001000 micrograph Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 231100000956 nontoxicity Toxicity 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 238000007415 particle size distribution analysis Methods 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 239000004332 silver Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000001308 synthesis method Methods 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 230000001988 toxicity Effects 0.000 description 1
- 231100000419 toxicity Toxicity 0.000 description 1
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- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/15—Nano-sized carbon materials
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- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
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Abstract
The invention discloses a starch carbon quantum dot and a preparation method and application thereof, wherein the method comprises the following steps: adding starch into distilled water, and stirring to obtain a starch solution; transferring the starch solution to a hydrothermal reaction kettle with a polytetrafluoroethylene lining for hydrothermal reaction; after the hydrothermal reaction is finished, cooling the hydrothermal reaction kettle to obtain a reaction solution; and centrifuging the reaction solution, removing the precipitate, filtering the centrifuged supernatant, and freeze-drying the obtained filtrate to obtain the starch carbon quantum dots. The invention provides a method for preparing starch carbon quantum dots by a one-step method, which has the advantages of simple preparation process, wide raw material source, simple operation, low production cost, easy industrial production and wide application in various fields such as biological medicine, food and the like, wherein the raw materials are only starch and water, and the starch carbon quantum dots have the function of inhibiting gram-positive bacteria and gram-negative bacteria.
Description
Technical Field
The invention belongs to the field of nano material preparation and bacteriostasis, and particularly relates to a starch carbon quantum dot and a preparation method and application thereof.
Background
The bacteriostatic nano material is a nano material with bacteriostatic function, and can effectively inhibit the growth and reproduction of microorganisms. Compared with the traditional bacteriostatic material, the bacteriostatic material has more excellent bacteriostatic performance due to the characteristic of nanometer size. For example, the bacteriostatic ability of the silver nano particles is far higher than that of antibacterial materials such as silver ions and the like. However, these nano antibacterial materials generally have toxicity, pose potential threats to human health and environment, and are cumbersome in manufacturing process and not suitable for mass production. Therefore, developing a nano antibacterial material with simple preparation process, environmental protection, no toxicity and no harm is the key point in the antibacterial field.
Carbon quantum dots, as a novel carbon nanomaterial, are carbon nanoparticles with a size of less than 10nm, and unlike conventional semiconductor quantum dots, do not cause environmental, health, and biotoxicity problems. The carbon quantum dots only consist of carbon, hydrogen, oxygen and nitrogen elements, so that the carbon quantum dots have extremely low cytotoxicity, good biocompatibility and excellent water solubility, and are wide in source and low in price. Therefore, the method is widely applied to various fields such as biological medicines, foods and the like.
The starch carbon quantum dots are carbon quanta prepared by taking starch as a raw material, the research on the functions of the carbon quanta is mainly focused on the fields of oxidation resistance, fluorescent probes and the like at present, and the research on the bacteriostatic function is rarely reported. Therefore, in order to further research the application and development of the starch carbon quantum dots with broad-spectrum bacteriostatic activity, a simple, easy, green and environment-friendly method for preparing the starch quantum dots needs to be developed, which can greatly improve the preparation and research efficiency of the starch carbon quantum dots, but no relevant research report on the preparation and bacteriostatic activity of the starch carbon quantum dots with bacteriostatic activity is found so far.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provides a preparation method of starch carbon quantum dots.
In order to achieve the purpose, the invention adopts the following technical scheme:
the invention provides a preparation method of starch carbon quantum dots, which comprises the following steps:
adding the starch solution into a hydrothermal reaction kettle with a polytetrafluoroethylene lining for hydrothermal reaction, and cooling the hydrothermal reaction kettle after the hydrothermal reaction is finished to obtain a reaction solution; and then centrifuging the reaction solution, removing the precipitate, finally filtering the centrifuged supernatant, and freeze-drying the obtained filtrate to obtain the starch carbon quantum dots.
According to the invention, starch is used as a raw material, the starch carbon quantum dots are prepared by a hydrothermal synthesis method without adding any chemical reagent, namely, the starch carbon quantum dots can be prepared by only one step, and the prepared starch carbon quantum dots have broad-spectrum antibacterial activity.
Preferably, adding starch into distilled water, and stirring to obtain the starch solution, wherein the weight of the starch is 2-8 g, and the volume of the distilled water is 100 mL; the stirring temperature is 40-60 ℃ and the stirring time is 1-3 hours.
Preferably, the reaction temperature of the hydrothermal reaction is 140-200 ℃, and the reaction time is 2-10 h.
Preferably, after the completion of the reaction, the hydrothermal reaction vessel is left at room temperature to be cooled.
Preferably, the centrifugal rotating speed during centrifugation is 8000-14000 rpm, the centrifugation time is 10-40 min, the centrifuged supernatant is filtered by a filter membrane, and the starch carbon quantum dots are obtained by a vacuum freeze drying method.
Preferably, the pore size of the filter is 0.45 um.
The invention also provides the starch carbon quantum dot prepared by the preparation method of the starch carbon quantum dot.
The invention also provides application of the starch carbon quantum dots to inhibition of gram-positive bacteria or gram-negative bacteria.
Preferably, the gram-positive bacterium is listeria monocytogenes or staphylococcus aureus.
Preferably, the gram-negative bacterium is escherichia coli or pseudomonas aeruginosa.
Compared with the prior art, the invention has the beneficial effects that:
the starch carbon quantum dots prepared by the method have simple preparation process, the raw materials are only starch and water, the diameter of the nano particles is 2.2-5.5nm, and the characteristics of the carbon quantum dots are met; the starch carbon quantum dot has the function of inhibiting the growth of gram-positive bacteria and gram-negative bacteria, the minimum inhibitory concentration is 2-3mg/mL, and the starch carbon quantum dot is indicated to be applicable to adjacent domains such as food, medical treatment and the like, and has wide market prospect. Compared with other synthesis methods, such as a microemulsion method, a thermal injection method and the like, the method for preparing the starch carbon quantum dots by the one-step method is simpler, more efficient and more green, the starch carbon quantum dots have the function of inhibiting gram-positive bacteria and gram-negative bacteria, and the preparation method has the advantages of wide raw material sources, simplicity in operation, low production cost, easiness in industrial production and wide application in various fields such as biological medicines, foods and the like.
The invention is further described below with reference to the accompanying drawings and specific embodiments.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings needed to be used in the description of the embodiments are briefly introduced below, and it is obvious that the drawings in the following description are some embodiments of the present invention, and it is obvious for those skilled in the art to obtain other drawings based on these drawings without creative efforts.
Fig. 1 is a schematic diagram of the synthesis process of starch carbon quantum dots in this example 1.
FIG. 2 is a transmission electron microscope image of the starch carbon quantum dots in example 1.
FIG. 3 is a high resolution TEM image of the starch carbon quantum dots of example 1.
Fig. 4 is a distribution diagram of the particle size of the starch carbon quantum dots in example 1.
FIG. 5 is the Oxford cup agar diffusion plot of the starch carbon quantum dots to Listeria monocytogenes (a), Staphylococcus aureus (b), Escherichia coli (c) and Pseudomonas aeruginosa (d) in this example 1.
FIG. 6 is a diagram of the detection of minimum inhibitory concentration of starch carbon quantum dots to Listeria monocytogenes (a), Staphylococcus aureus (b), Escherichia coli (c) and Pseudomonas aeruginosa (d) in this example 1.
Fig. 7 shows the bacteriostatic diameter of starch carbon quantum dots to listeria monocytogenes under different preparation conditions, (a) shows the bacteriostatic diameter of starch carbon quantum dots to listeria monocytogenes of example 2, and (b) shows the bacteriostatic diameter of starch carbon quantum dots to listeria monocytogenes of example 3.
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 some, not all, embodiments of the present invention. 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
The embodiment is a method for preparing starch quantum dots, and the method comprises the following specific steps:
s1, 6g of starch is weighed into a beaker, 100mL of distilled water is added, and the mixture is stirred for 1 hour at 55 ℃ to obtain a starch solution.
And S2, transferring the starch solution to a hydrothermal reaction kettle with a polytetrafluoroethylene lining for reaction at 180 ℃ for 6 hours, cooling the hydrothermal reaction kettle at room temperature after the hydrothermal reaction is finished, and opening the hydrothermal reaction kettle after cooling to obtain a brown solution.
S3, centrifuging the brown solution at 10000rpm for 30min, discarding the precipitate, filtering the centrifuged supernatant with a 0.45um filter membrane, and freeze-drying the obtained filtrate to obtain the starch carbon quantum dots, wherein the preparation process is schematically shown in figure 1.
The starch carbon quantum dots obtained in the example were subjected to transmission electron microscope, high-resolution transmission electron microscope and particle size distribution analysis.
The diameter of the starch carbon nano particle is found to be 2.2-5.5nm by a transmission electron microscope, a high-resolution transmission electron microscope and particle size distribution molecules, which accords with the characteristics of the carbon quantum dot, and is shown in figures 2-4.
The bacteriostatic activity and the minimum bacteriostatic concentration of the starch carbon quantum dots obtained in the embodiment are evaluated, and the evaluation specifically comprises the following steps:
agar diffusion bacteriostasis experiments are carried out on the prepared starch carbon quantum dots to Listeria monocytogenes, staphylococcus aureus, escherichia coli and pseudomonas aeruginosa, and the starch carbon quantum dots are found to have good inhibition effects on the four bacteria (figure 5), and the minimum bacteriostasis concentrations are respectively 3mg/mL, 2mg/mL and 2mg/mL (figure 6).
Example 2
The embodiment is a method for preparing starch quantum dots, and the method comprises the following specific steps:
s1, weighing 8g of starch in a beaker, adding 100mL of distilled water, and stirring at 55 ℃ for 2 hours to obtain a starch solution.
And S2, transferring the starch solution to a hydrothermal reaction kettle with a polytetrafluoroethylene lining for reaction, reacting for 4 hours at 200 ℃, after the hydrothermal reaction is finished, cooling the hydrothermal reaction kettle at room temperature, and opening the hydrothermal reaction kettle after cooling to obtain a brown solution.
S3, centrifuging the brown solution at 10000rpm for 30min, discarding the precipitate, filtering the centrifuged supernatant with a 0.45um filter membrane, and freeze-drying the obtained filtrate to obtain the starch carbon quantum dots.
The bacteriostatic activity of the starch carbon quantum dots obtained in the embodiment is evaluated, and specifically:
the prepared starch carbon quantum dots are subjected to an agar diffusion bacteriostasis experiment on listeria monocytogenes, and the bacteriostasis diameters of the starch carbon quantum dots to the listeria monocytogenes are found to be 20.21mm respectively (fig. 7).
Example 3
The embodiment is a method for preparing starch quantum dots, and the method comprises the following specific steps:
s1, weighing 4g of starch in a beaker, adding 100mL of distilled water, and stirring at 55 ℃ for 1 hour to obtain a starch solution.
And S2, transferring the starch solution to a hydrothermal reaction kettle with a polytetrafluoroethylene lining for reaction, reacting for 8 hours at 160 ℃, after the hydrothermal reaction is finished, cooling the hydrothermal reaction kettle at room temperature, and opening the hydrothermal reaction kettle after cooling to obtain a brown solution.
S3, centrifuging the brown solution at 10000rpm for 30min, discarding the precipitate, filtering the centrifuged supernatant with a 0.45um filter membrane, and freeze-drying the obtained filtrate to obtain the starch carbon quantum dots.
The bacteriostatic activity of the starch carbon quantum dots obtained in the embodiment is evaluated, and specifically:
the prepared starch carbon quantum dots are subjected to an agar diffusion bacteriostasis experiment on listeria monocytogenes, and the bacteriostasis diameters of the starch carbon quantum dots to the listeria monocytogenes are found to be 18.91mm respectively (fig. 7).
While the invention has been described with reference to specific embodiments, the invention is not limited thereto, and various equivalent modifications and substitutions can be easily made by those skilled in the art within the technical scope of the invention. Therefore, the protection scope of the present invention shall be subject to the protection scope of the claims.
Claims (10)
1. The preparation method of the starch carbon quantum dot is characterized by comprising the following steps:
adding the starch solution into a hydrothermal reaction kettle with a polytetrafluoroethylene lining for hydrothermal reaction, and cooling the hydrothermal reaction kettle after the hydrothermal reaction is finished to obtain a reaction solution; and then centrifuging the reaction solution, removing the precipitate, finally filtering the centrifuged supernatant, and freeze-drying the obtained filtrate to obtain the starch carbon quantum dots.
2. The preparation method of the starch carbon quantum dot according to claim 1, wherein starch is added into distilled water and stirred to obtain the starch solution, wherein the weight of the starch is 2-8 g, and the volume of the distilled water is 100 mL; the stirring temperature is 40-60 ℃ and the stirring time is 1-3 hours.
3. The method for preparing the starch carbon quantum dots according to claim 1, wherein the reaction temperature of the hydrothermal reaction is 140-200 ℃ and the reaction time is 2-10 h.
4. The method for preparing the starch carbon quantum dots according to claim 1, wherein after the reaction is finished, the hydrothermal reaction kettle is placed at room temperature for cooling.
5. The preparation method of the starch carbon quantum dot according to claim 1, wherein the centrifugal rotation speed during centrifugation is 8000-14000 rpm, the centrifugation time is 10-40 min, the centrifuged supernatant is filtered by a filter membrane, and the starch carbon quantum dot is obtained by a vacuum freeze drying method.
6. The method for preparing starch carbon quantum dots according to claim 5, wherein the pore size of the filter membrane is 0.45 um.
7. The starch carbon quantum dot prepared by the preparation method of the starch carbon quantum dot according to any one of claims 1 to 6.
8. Use of the starch carbon quantum dots according to claim 7 for inhibiting gram-positive bacteria or gram-negative bacteria.
9. The use according to claim 8, wherein the gram-positive bacterium is Listeria monocytogenes or Staphylococcus aureus.
10. Use according to claim 8, wherein the gram-negative bacteria are Escherichia coli or Pseudomonas aeruginosa.
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| CN115744878A (en) * | 2022-11-14 | 2023-03-07 | 兰州大学 | Fluorescent coffee grounds carbon quantum dots and preparation method and application thereof |
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| CN108300464A (en) * | 2018-04-17 | 2018-07-20 | 南京师范大学 | It is a kind of can preparation method and products thereof of N doping carbon quantum dots of antibacterial, application |
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| CN108300464A (en) * | 2018-04-17 | 2018-07-20 | 南京师范大学 | It is a kind of can preparation method and products thereof of N doping carbon quantum dots of antibacterial, application |
| CN109292753A (en) * | 2018-12-06 | 2019-02-01 | 洛阳师范学院 | A kind of carbon quantum dot and its environment-friendly preparation method thereof and application |
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| CN115744878B (en) * | 2022-11-14 | 2024-07-12 | 兰州大学 | Fluorescent coffee grounds carbon quantum dot and preparation method and application thereof |
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