CN115744878B - Fluorescent coffee grounds carbon quantum dot and preparation method and application thereof - Google Patents
Fluorescent coffee grounds carbon quantum dot and preparation method and application thereof Download PDFInfo
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Abstract
The invention belongs to the technical field of antibacterial nano materials, and particularly relates to a fluorescent coffee grounds carbon quantum dot and a preparation method and application thereof. The method comprises the following steps: dispersing coffee grounds as precursor substances in water, stirring, uniformly dispersing by ultrasonic, performing hydrothermal reaction at 150-180 ℃, centrifuging after the reaction is finished to obtain supernatant, and filtering to obtain the coffee grounds carbon quantum dots. According to the invention, the coffee grounds are prepared into the carbon quantum dot nano material to form the nano material which has antibacterial activity, excellent fluorescence performance and selective antibacterial property, and the coffee grounds carbon quantum dots are used as a main substrate to prepare antibacterial products, so that the coffee grounds have good water solubility and dispersibility, are favorable for the materials to be used in a biological system or mixed with other materials, have low toxicity, and can be suitable for environments in which ethanol preparations or other antibacterial preparations with high toxicity cannot be selected.
Description
Technical Field
The invention belongs to the technical field of antibacterial nano materials, and particularly relates to a fluorescent coffee grounds carbon quantum dot and a preparation method and application thereof.
Background
In the processes of nosocomial infection, food preservation and disease progression, the existence and reproduction of pathogenic bacteria are one of the important factors causing adverse consequences. The adverse effects of bacteria can be effectively controlled by antibiotics, such as penicillin, cephalosporin, etc., but due to the presence of bacterial drug resistance mutations, e.g. partially mutated gram-negative bacteria with an ultra-broad spectrum of beta-lactamases can hydrolyse antibiotics to exhibit drug resistance, resulting in the necessity to limit the use of traditional antibiotics and to seek effective alternatives. The existing physical methods, such as ultraviolet irradiation, cannot inhibit the growth and reproduction of bacteria for a long time; in the chemical method, such as glutaraldehyde, the toxic effect limited by substances is not suitable for directly acting in human bodies, and the food is bacteriostatic and can only be applied to partial environment and instrument disinfection; in the prior material angle solutions, for example, copper ion coatings inhibit bacterial growth and reproduction on metal surfaces, and are effective for a long time but are widely used for building materials; the traditional antibiotic has excellent antibacterial performance, but because of broad-spectrum bacteriostasis, the mutation of non-targeted bacterial drug resistance is promoted, and therefore, the development of the antibacterial nano material with lasting bacteriostasis, small cytotoxicity, strong universality and selective bacteriostasis has important significance.
The precursors of bacteriostatic nanomaterials can be separated from sources into two, one derived from a single synthetic substance and the other from a naturally occurring plant or extract thereof. The two main differences are in development difficulty and material composition, the artificially synthesized materials need more repeated modification designs, the components are relatively single, the development period is long, the mechanism is generally clear and obvious, the effect is obvious, a plurality of natural active compounds and vitamin synergistic combinations exist in the naturally-existing extracts, the natural active compounds and vitamin synergistic combinations have wide activity, the development period is short, meaningful indexes are easily observed so as to be convenient for providing hypothesis, therefore, for rapidly developing the antibacterial material meeting the requirements, the plants or the extracts with related activity verification are ideal precursors of the material.
The carbon quantum dots are paid more attention to the field of biological medicine compared with other carbon nano materials containing metal elements and traditional carbon nano materials because of biocompatibility, fluorescence performance, chemical stability and easy surface modification, and are applied to material detection, biological imaging, catalysis, medicine carrying and the like. The antibacterial activity of the carbon quantum dots has attracted a great deal of attention in recent years, and the interaction with microorganisms depends on the composition, the size, the shape and the surface active groups of the carbon quantum dots, and is mainly classified into cationic carbon quantum dots, carbon quantum dots with special shapes, photodynamic carbon quantum dots, antibiotic modified carbon quantum dots and the like according to antibacterial mechanisms, wherein the antibiotic modified carbon quantum dots have the best effect, but are limited by drug resistance mutation of bacteria, cannot be widely used, and cannot selectively inhibit bacteria.
The coffee industry is a key component of global economy, with by-products in production exceeding 20 million tons per year, such as coffee grounds, but the by-products are often discarded directly and not utilized directly. Therefore, development of antibacterial materials for waste coffee grounds has important significance in solving the problem of bacteriostasis and the problem of utilization of coffee byproducts.
Disclosure of Invention
In order to solve the problems, the invention provides the fluorescent coffee grounds carbon quantum dots, the preparation method and the application thereof, and the coffee grounds are prepared into the carbon quantum dots nano-material to form the nano-material which has antibacterial activity and excellent fluorescence performance and can selectively inhibit bacteria, and the coffee grounds carbon quantum dots are used as a main substrate to prepare antibacterial products, so that the fluorescent coffee grounds carbon quantum dots have good water solubility and dispersibility, are favorable for being used in biological systems or being mixed with other materials, have lower toxicity, can be suitable for environments in which ethanol preparations or other antibacterial preparations with larger toxicity cannot be selected, and have good application prospects.
The invention solves the technical problems through the following technical proposal.
The first object of the invention is to provide a preparation method of fluorescent coffee grounds carbon quantum dots, which comprises the following steps:
Dispersing coffee grounds as precursor substances in water, stirring, uniformly dispersing by ultrasonic, performing hydrothermal reaction at 150-180 ℃, centrifuging after the reaction is finished to obtain supernatant, and filtering to obtain the coffee grounds carbon quantum dots.
Preferably, the mass volume ratio of the coffee grounds to the water is 1g: 30-100 mL.
Preferably, the stirring is magnetic stirring for 10-15 min and the ultrasonic time for 15-30 min.
Preferably, the hydrothermal reaction time is 5-8 hours.
Preferably, the rotational speed of the centrifugation is 8000-10000 r/min, and the time is 5-10 min; filtration was performed using 0.22 μm MCE.
The second object of the invention is to provide the fluorescent coffee grounds carbon quantum dots prepared by the preparation method.
The third object of the invention is to provide an application of the fluorescent coffee grounds carbon quantum dots in preparing a selective antibacterial product.
Preferably, the fluorescent coffee grounds carbon quantum dots selectively inhibit staphylococcus aureus.
Preferably, the antibacterial product comprises a spray antibacterial agent, an antibacterial preservative film and an antibacterial dressing.
Compared with the prior art, the invention has the following beneficial effects:
(1) The fluorescent coffee grounds carbon quantum dots are prepared by adopting a one-step hydrothermal method, the preparation method is simple, the precursor substance of the carbon quantum dots is coffee grounds, the waste is utilized, the cost is low, the source is wide, and the coffee grounds are prepared into the carbon quantum dots nano material, so that the nano material with antibacterial activity, excellent fluorescent performance and selective bacteriostasis is formed.
(2) The fluorescent coffee grounds carbon quantum dots prepared by the invention have good fluorescence performance, can realize the monitoring of the concentration of the carbon quantum dots in bacteriostatic products, have good water solubility and dispersibility, are favorable for materials to be used in biological systems or mixed in other materials, have lower toxicity, can be suitable for environments in which ethanol preparations or other bacteriostatic preparations with higher toxicity cannot be selected, and have wide application prospects.
Drawings
FIG. 1 is a graph showing fluorescence emission spectra of carbon quantum dots of coffee grounds prepared in example 1 of the present invention;
FIG. 2 is a life chart of the carbon quantum dots of coffee grounds prepared in example 1 of the present invention;
FIG. 3 is a Fourier infrared plot of the carbon quantum dots of coffee grounds prepared in example 1 of the present invention;
FIG. 4 is a transmission electron microscope image of the coffee grounds carbon quantum dots prepared in example 1 of the present invention;
FIG. 5 is an electron diffraction pattern of the coffee grounds carbon quantum dots provided by the embodiment of the invention;
FIG. 6 is a graph showing the bacteriostatic effect of the coffee grounds carbon quantum dots of example 1 on Staphylococcus aureus;
Fig. 7 is a graph showing the antibacterial effect of the coffee grounds carbon quantum dots of example 1 on escherichia coli.
Detailed Description
The following description of the embodiments of the present invention will be made clearly and completely with reference to the accompanying drawings, in which it is apparent that the embodiments described are only some embodiments of the present invention, but not all embodiments. All other embodiments, based on the embodiments of the invention, which a person of ordinary skill in the art would obtain without making inventive faculty, are within the scope of the invention.
It should be noted that the technical terms used in the present invention are only for describing specific embodiments, and are not intended to limit the scope of the present invention, and various raw materials, reagents, instruments and equipment used in the following embodiments of the present invention may be purchased commercially or prepared by existing methods unless otherwise specifically described.
Example 1
A preparation method of fluorescent coffee grounds carbon quantum dots comprises the following steps:
Removing impurities from waste coffee grounds, putting the waste coffee grounds into a crucible, drying at 60 ℃, weighing 1g of the coffee grounds with the impurities removed as precursor substances, dispersing the precursor substances into 60mL of deionized water, magnetically stirring the precursor substances for 10min, putting the precursor substances into an ultrasonic cleaner, performing ultrasonic treatment for 30min to uniformly disperse the precursor substances, transferring the uniformly mixed solution into a 100mL high-pressure reaction kettle, performing hydrothermal reaction at 180 ℃ of an oven for 5h, cooling to room temperature after the reaction is finished, taking out the product, centrifuging the product for 10min at 8000r/min, extracting supernatant, filtering the supernatant by a 0.22 mu m MCE injector, obtaining a solution of coffee carbon quantum dots, and storing the solution at 4-6 ℃.
To illustrate the performance of the fluorescent coffee grounds carbon quantum dots provided by the present invention, the fluorescent coffee grounds carbon quantum dots provided in example 1 were tested.
FIG. 1 is a graph showing fluorescence emission spectra of carbon quantum dots of coffee grounds prepared in example 1 of the present invention. As shown in FIG. 1, under the condition of excitation light wavelength of 360nm, the emitted light with fluorescence intensity of 900 exists at 440nm, the Stokes shift of 80nm exists, the peak shape is smooth and sharp, and the peak value is obvious. .
Fig. 2 is a life chart of the coffee grounds carbon quantum dots prepared in example 1 of the present invention. As shown in FIG. 2, τ1 is 0.8541ns, τ2 is 3.741ns, and τ3 is 13.8195ns.
Fig. 3 is a fourier infrared plot of the coffee grounds carbon quantum dots prepared in example 1 of the present invention. As shown in fig. 3, among the six more prominent absorption peaks, the absorption peak at 3383cm -1 may be attributed to an O-H stretching vibration peak, the absorption peak at 2930cm -1 may be attributed to a C-H stretching vibration peak, the absorption peak at 1768cm -1 may be attributed to a-COOH stretching vibration peak, the absorption peak at 1632cm -1 may be attributed to a c=o stretching vibration peak, the absorption peak at 1402cm -1 may be attributed to a-C-OH stretching vibration peak, and the absorption peak at 1070cm -1 may be attributed to a C-O-C stretching vibration peak.
Fig. 4 is a transmission electron microscope image of the coffee grounds carbon quantum dots prepared in example 1 of the present invention. As shown in FIG. 4, the obtained nanomaterial is lamellar, and is occasionally aggregated into irregular black agglomerate-shaped substances, and the particle size is varied from 10 nm to 100 nm.
Fig. 5 is an electron diffraction diagram of the carbon quantum dots of the coffee grounds provided by the embodiment of the invention. As shown in FIG. 5, the electron diffraction pattern under the electron microscope has diffraction spots and diffraction rings, and the spot group is parallelogram and is a core-shell structure characteristic. .
EXAMPLE 2 bacteriostasis test of Staphylococcus aureus
The coffee grounds carbon quantum dots prepared in example 1 were tested for their ability to inhibit staphylococcus aureus (gram positive bacteria), comprising the steps of:
placing 10ul of preserved staphylococcus aureus bacterial liquid in 5mL of 3g/100mL of pancreatic protein culture liquid, and culturing at constant temperature for 10 hours to recover strains to form a bacterial liquid for later use;
The cultured staphylococcus aureus bacterial liquid is selected, diluted in the proportion of 1:10 5, 100 mu L of bacterial suspension and 200 mu L of coffee grounds carbon quantum dots prepared in the embodiment 1 are added into a culture dish, the culture dish is poured into a high-pressure steam sterilized benard-parker agar (BP) culture medium to be uniformly mixed, the coffee grounds carbon quantum dots prepared in the embodiment 1 are not added as blank control, and the colony count is observed after the culture in a constant-temperature incubator at 37 ℃ for 24 hours.
Fig. 6 is a graph showing the bacteriostatic effect of the coffee grounds carbon quantum dots of example 1 on staphylococcus aureus. As shown in fig. 6, the coffee grounds carbon quantum dots of example 1 have a significant inhibitory effect on the staphylococcus aureus population.
Example 3 bacteriostasis test of E.coli
Taking 10ul of preserved escherichia coli strain bacterial liquid, placing in 5mL of 1.8g/100mL nutrient agar culture liquid, and carrying out shaking culture at constant temperature for 10h to recover the bacterial strain to form standby bacterial liquid;
The method comprises the steps of selecting a bacterial solution of a cultured escherichia coli strain, diluting the bacterial solution in a ratio of 1:10 5, adding 100 mu l of bacterial suspension and 200 mu l of coffee grounds carbon quantum dots of example 1 into a culture dish, pouring nutrient agar culture medium, uniformly mixing, taking the coffee grounds carbon quantum dots prepared in example 1 as a blank control, culturing in a constant-temperature incubator at 37 ℃ for 24 hours, and observing the colony number.
Fig. 7 is a graph showing the antibacterial effect of the coffee grounds carbon quantum dots of example 1 on escherichia coli. As shown in fig. 7, the coffee grounds carbon quantum dots of example 1 did not have a significant inhibitory effect on escherichia coli.
Example 5
A trauma and mucosa antibacterial spray preparation, comprising the following steps:
50mg of the coffee grounds carbon quantum dots in the example 1 are dissolved in 1000mL of water, 2.5g of menthol, 2g of borneol, 3.5g of aspartame, 2.5g of potassium sorbate, 2.5g of citric acid, 2.5g of sodium alginate and 0.2g of calcium chloride are added, and after uniform stirring, filtration and filling are carried out, thus obtaining the antibacterial spray preparation applicable to mucous membranes and skin.
Example 6
A trauma antibacterial ointment preparation is prepared from the following components in parts by weight:
1-5 parts of coffee grounds carbon quantum dots of the embodiment 1, 5-10 parts of vitamin E, 1-5 parts of rose essential oil, 1-5 parts of rhizoma corydalis, 3-5 parts of myrrh, 3-10 parts of pearl powder, 1-3 parts of borneol, 0.1-1 part of rosemary and 30-60 parts of vaseline.
Weighing the components, mixing uniformly at a low temperature below 60 ℃, and preparing the selective antibacterial ointment.
It should be noted that, when numerical ranges are referred to in the present invention, it should be understood that two endpoints of each numerical range and any numerical value between the two endpoints are optional, and because the adopted step method is the same as the embodiment, in order to prevent redundancy, the present invention describes a preferred embodiment. While preferred embodiments of the present invention have been described, additional variations and modifications in those embodiments may occur to those skilled in the art once they learn of the basic inventive concepts. It is therefore intended that the following claims be interpreted as including the preferred embodiments and all such alterations and modifications as fall within the scope of the invention.
It will be apparent to those skilled in the art that various modifications and variations can be made to the present invention without departing from the spirit or scope of the invention. Thus, it is intended that the present invention also include such modifications and alterations insofar as they come within the scope of the appended claims or the equivalents thereof.
Claims (2)
1. The application of the fluorescent coffee grounds carbon quantum dots in preparing the products for selectively inhibiting staphylococcus aureus is characterized by comprising the following steps:
dispersing coffee grounds as precursor substances in water, magnetically stirring for 10min, uniformly dispersing by ultrasonic for 30min, performing hydrothermal reaction at 180 ℃ for 5h, centrifuging after the reaction is finished to obtain supernatant, and filtering to obtain coffee grounds carbon quantum dots;
the mass volume ratio of the coffee grounds to the water is 1g:60mL;
The rotational speed of the centrifugation is 8000r/min, and the time is 10min; filtration was performed using 0.22 μm MCE.
2. The use according to claim 1, wherein the bacteriostatic product comprises a spray bacteriostatic agent, a bacteriostatic preservative film, a bacteriostatic dressing.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202211421754.5A CN115744878B (en) | 2022-11-14 | Fluorescent coffee grounds carbon quantum dot and preparation method and application thereof |
Applications Claiming Priority (1)
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| CN106629658A (en) * | 2016-11-12 | 2017-05-10 | 兰州大学 | Preparation method of fluorescent carbon quantum dot |
| CN111909691A (en) * | 2020-06-23 | 2020-11-10 | 南京师范大学 | Preparation method of photo-thermal antibacterial near-infrared carbon quantum dots, product and application thereof |
| CN114105121A (en) * | 2021-11-01 | 2022-03-01 | 浙江省农业科学院 | Starch carbon quantum dot and preparation method and application thereof |
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| CN106629658A (en) * | 2016-11-12 | 2017-05-10 | 兰州大学 | Preparation method of fluorescent carbon quantum dot |
| CN111909691A (en) * | 2020-06-23 | 2020-11-10 | 南京师范大学 | Preparation method of photo-thermal antibacterial near-infrared carbon quantum dots, product and application thereof |
| CN114105121A (en) * | 2021-11-01 | 2022-03-01 | 浙江省农业科学院 | Starch carbon quantum dot and preparation method and application thereof |
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