CN114561205B - Eutectic solvent modified carbon quantum dot and preparation method and application thereof - Google Patents
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- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical class C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 title claims abstract description 70
- 230000005496 eutectics Effects 0.000 title claims abstract description 64
- 239000002904 solvent Substances 0.000 title claims abstract description 63
- 238000002360 preparation method Methods 0.000 title claims abstract description 24
- AEMRFAOFKBGASW-UHFFFAOYSA-N Glycolic acid Chemical compound OCC(O)=O AEMRFAOFKBGASW-UHFFFAOYSA-N 0.000 claims abstract description 35
- WXMKPNITSTVMEF-UHFFFAOYSA-M sodium benzoate Chemical compound [Na+].[O-]C(=O)C1=CC=CC=C1 WXMKPNITSTVMEF-UHFFFAOYSA-M 0.000 claims abstract description 32
- 235000010234 sodium benzoate Nutrition 0.000 claims abstract description 32
- 239000004299 sodium benzoate Substances 0.000 claims abstract description 32
- 238000001514 detection method Methods 0.000 claims abstract description 24
- 241001070941 Castanea Species 0.000 claims abstract description 19
- 235000014036 Castanea Nutrition 0.000 claims abstract description 19
- TVXBFESIOXBWNM-UHFFFAOYSA-N Xylitol Natural products OCCC(O)C(O)C(O)CCO TVXBFESIOXBWNM-UHFFFAOYSA-N 0.000 claims abstract description 19
- HEBKCHPVOIAQTA-UHFFFAOYSA-N meso ribitol Natural products OCC(O)C(O)C(O)CO HEBKCHPVOIAQTA-UHFFFAOYSA-N 0.000 claims abstract description 19
- HEBKCHPVOIAQTA-SCDXWVJYSA-N xylitol Chemical compound OC[C@H](O)[C@@H](O)[C@H](O)CO HEBKCHPVOIAQTA-SCDXWVJYSA-N 0.000 claims abstract description 19
- 229960002675 xylitol Drugs 0.000 claims abstract description 19
- 235000010447 xylitol Nutrition 0.000 claims abstract description 19
- 239000000811 xylitol Substances 0.000 claims abstract description 19
- 239000007788 liquid Substances 0.000 claims abstract description 13
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 12
- 238000002156 mixing Methods 0.000 claims abstract description 11
- 239000000843 powder Substances 0.000 claims abstract description 11
- 238000001914 filtration Methods 0.000 claims abstract description 10
- 239000008367 deionised water Substances 0.000 claims abstract description 8
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 8
- 239000000706 filtrate Substances 0.000 claims abstract description 7
- 238000010438 heat treatment Methods 0.000 claims abstract description 7
- 238000000034 method Methods 0.000 claims description 18
- 239000012528 membrane Substances 0.000 claims description 6
- 239000000523 sample Substances 0.000 claims description 5
- 238000001471 micro-filtration Methods 0.000 claims description 4
- 239000002245 particle Substances 0.000 claims description 3
- 238000004519 manufacturing process Methods 0.000 claims 1
- 235000013305 food Nutrition 0.000 abstract description 11
- 239000002994 raw material Substances 0.000 abstract description 7
- 239000000463 material Substances 0.000 abstract description 3
- 239000003755 preservative agent Substances 0.000 description 8
- 230000000052 comparative effect Effects 0.000 description 6
- 230000002335 preservative effect Effects 0.000 description 6
- 238000012360 testing method Methods 0.000 description 5
- 235000019249 food preservative Nutrition 0.000 description 3
- 239000005452 food preservative Substances 0.000 description 3
- 238000010791 quenching Methods 0.000 description 3
- 230000000171 quenching effect Effects 0.000 description 3
- 239000006228 supernatant Substances 0.000 description 3
- 238000003917 TEM image Methods 0.000 description 2
- 235000013373 food additive Nutrition 0.000 description 2
- 239000002778 food additive Substances 0.000 description 2
- 238000004128 high performance liquid chromatography Methods 0.000 description 2
- 238000004321 preservation Methods 0.000 description 2
- 241000283690 Bos taurus Species 0.000 description 1
- 241000207199 Citrus Species 0.000 description 1
- 206010028980 Neoplasm Diseases 0.000 description 1
- 206010067482 No adverse event Diseases 0.000 description 1
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 description 1
- 241000353135 Psenopsis anomala Species 0.000 description 1
- 244000294611 Punica granatum Species 0.000 description 1
- 235000014360 Punica granatum Nutrition 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 230000000844 anti-bacterial effect Effects 0.000 description 1
- 244000052616 bacterial pathogen Species 0.000 description 1
- 230000008033 biological extinction Effects 0.000 description 1
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- 201000011510 cancer Diseases 0.000 description 1
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- 238000002474 experimental method Methods 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
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- 238000002189 fluorescence spectrum Methods 0.000 description 1
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- 230000002401 inhibitory effect Effects 0.000 description 1
- 230000000670 limiting effect Effects 0.000 description 1
- 238000012417 linear regression Methods 0.000 description 1
- 210000004185 liver Anatomy 0.000 description 1
- 230000002503 metabolic effect Effects 0.000 description 1
- 244000005700 microbiome Species 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000003607 modifier Substances 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 235000019449 other food additives Nutrition 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 235000021067 refined food Nutrition 0.000 description 1
- 235000014102 seafood Nutrition 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 238000007873 sieving Methods 0.000 description 1
- 238000002798 spectrophotometry method Methods 0.000 description 1
- 230000001954 sterilising effect Effects 0.000 description 1
- 238000004659 sterilization and disinfection Methods 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
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- 230000002459 sustained effect Effects 0.000 description 1
- 238000004809 thin layer chromatography Methods 0.000 description 1
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- C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
- C09K11/02—Use of particular materials as binders, particle coatings or suspension media therefor
- C09K11/025—Use of particular materials as binders, particle coatings or suspension media therefor non-luminescent particle coatings or suspension media
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- B82Y20/00—Nanooptics, e.g. quantum optics or photonic crystals
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- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- C09K11/65—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing carbon
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- G01N21/62—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
- G01N21/63—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light optically excited
- G01N21/64—Fluorescence; Phosphorescence
- G01N21/6428—Measuring fluorescence of fluorescent products of reactions or of fluorochrome labelled reactive substances, e.g. measuring quenching effects, using measuring "optrodes"
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
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- G01N21/63—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light optically excited
- G01N21/64—Fluorescence; Phosphorescence
- G01N21/6428—Measuring fluorescence of fluorescent products of reactions or of fluorochrome labelled reactive substances, e.g. measuring quenching effects, using measuring "optrodes"
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Abstract
The invention relates to the technical field of carbon quantum dot materials, and particularly discloses a eutectic solvent modified carbon quantum dot, and a preparation method and application thereof. The preparation method of the eutectic solvent modified carbon quantum dot comprises the following steps: a. mixing chestnut skin powder and a natural eutectic solvent of glycollic acid/xylitol, adding deionized water, uniformly mixing, centrifuging, and filtering to obtain clear liquid; b. and heating the clear liquid to perform a hydrothermal reaction, and centrifuging and filtering after the hydrothermal reaction is completed to obtain a filtrate, wherein the filtrate is the eutectic solvent modified carbon quantum dots. The eutectic solvent modified carbon quantum dot provided by the invention can realize rapid qualitative and quantitative detection of sodium benzoate, and has the advantages of simple preparation method, wide raw material sources, low preparation cost, short detection period, nature and no pollution, and can realize rapid detection of sodium benzoate in a large amount of foods.
Description
Technical Field
The invention relates to the technical field of carbon quantum dot materials, in particular to a eutectic solvent modified carbon quantum dot, and a preparation method and application thereof.
Background
Food preservatives are agents that inhibit food spoilage and have a sustained inhibitory effect on the growth of microorganisms that use spoilage substances as metabolic substrates. The food preservative can inhibit food spoilage under different conditions, and has continuous antibacterial effect especially under the condition of insufficient general sterilization. Therefore, preservatives and other food additives are added to many processed foods, which has become unavoidable. However, excessive amounts of food additives can have irreparable consequences for the body, especially preservatives. However, if no preservative is used in some foods, a large amount of pathogenic bacteria can be caused to grow in a short time. Therefore, the addition of a proper amount and a small amount of preservative is unavoidable. However, there are many foods on the market to which an excessive amount of preservative, such as sodium benzoate, is added for preservation, and are widely used for preservation of various seafood products. Sodium benzoate is a typical preservative, and small amounts of sodium benzoate are metabolized by the human body and do not cause damage to the human body, but excessive intake can cause harm to the human liver and even cause cancer, so that sodium benzoate needs to be strictly detected in food applications.
The main methods for detecting sodium benzoate in food at present are as follows: high performance liquid chromatography, thin layer chromatography, spectrophotometry, etc. The high performance liquid chromatography is the most commonly used method and is also the first method of national standards. However, the existing detection method has a plurality of problems, including: the single-wavelength gradient elution ultraviolet detection mode is used for separation detection in detection, sample pretreatment is complex, time-consuming, labor-consuming and reagent-consuming, detection efficiency is low, working strength of staff is high, working efficiency is low, and the method is not suitable for mass sample detection.
Disclosure of Invention
Aiming at the problems of the prior method for detecting preservative sodium benzoate in food, the invention provides a eutectic solvent modified carbon quantum dot, a preparation method and application thereof, wherein the eutectic solvent modified carbon quantum dot can realize rapid qualitative and quantitative detection of sodium benzoate, and the preparation method is simple, wide in raw material source, low in preparation cost, short in detection period, natural and pollution-free, and can realize rapid detection of sodium benzoate in a large quantity of food.
In order to achieve the above purpose, the embodiment of the invention adopts the following technical scheme:
the preparation method of the eutectic solvent modified carbon quantum dot comprises the following steps:
a. mixing chestnut skin powder and a natural eutectic solvent of glycollic acid/xylitol, adding deionized water, uniformly mixing, centrifuging, and filtering to obtain clear liquid;
b. and heating the clear liquid to perform a hydrothermal reaction, and centrifuging and filtering after the hydrothermal reaction is completed to obtain a filtrate, wherein the filtrate is the eutectic solvent modified carbon quantum dots.
Compared with the prior art, the preparation method of the carbon quantum dot modified by the eutectic solvent is simple, the natural chestnut skin is used as a raw material, and the glycolic acid/xylitol natural eutectic solvent is used as a modifier, so that the obtained carbon quantum dot has good environmental compatibility and no toxic effect. The carbon quantum dot prepared by the raw materials and the method has extremely high fluorescence intensity, and can realize the response to the extinction of sodium benzoate in the food additive, so that the carbon quantum dot material can be applied to the field of food detection for the first time. Meanwhile, the method for detecting sodium benzoate by using the carbon quantum dots prepared by the method is simple to operate, has high response speed, is favorable for on-site detection, has good application prospect, and has great significance for the development of the food safety detection field.
Preferably, in the step a, the particle size of the chestnut skin powder is less than or equal to 0.15mm.
Preferably, in the step a, the preparation method of the natural eutectic solvent of the glycollic acid/the xylitol comprises the following steps: mixing glycolic acid and xylitol according to a molar ratio of 2-4:1, and heating to 70-120 ℃ until transparent uniform liquid is formed, wherein the liquid is the natural eutectic solvent of the glycolic acid/the xylitol.
Preferably, in the step a, the mass ratio of the chestnut skin powder to the glycolic acid/xylitol natural eutectic solvent is 1:8-12.
The mass ratio of the chestnut skin powder to the glycolic acid/xylitol natural eutectic solvent can further improve the fluorescence intensity of the obtained carbon quantum dots.
Preferably, in the step a, the mass volume ratio of the chestnut shell powder to the deionized water is 1g:450-550mL.
Preferably, in the step b, the temperature of the hydrothermal reaction is 200-220 ℃ and the time is 10-11 h.
The temperature and time of the hydrothermal reaction can further improve the uniformity of the prepared carbon quantum dots and reduce the granularity of the prepared carbon quantum dots.
Preferably, in step a and step b, the filtration membrane is a microfiltration membrane of 0.22 μm.
The invention also provides the eutectic solvent modified carbon quantum dot prepared by the preparation method of the eutectic solvent modified carbon quantum dot.
The invention also provides the eutectic solvent modified carbon quantum dot prepared by the preparation method of the eutectic solvent modified carbon quantum dot.
The invention also provides application of the eutectic solvent modified carbon quantum dot in a fluorescence detection probe serving as sodium benzoate.
Drawings
FIG. 1 is a TEM image of the eutectic solvent modified carbon quantum dots prepared in example 1 of the present invention;
FIG. 2 is a graph showing the comparison of fluorescence intensity of the eutectic solvent modified carbon quantum dots prepared in example 1 of the present invention at different excitation wavelengths;
FIG. 3 is a graph showing the comparison of fluorescence intensity of different carbon quantum dots detected in test example 1 of the present invention;
FIG. 4 is a graph showing the comparative response of eutectic solvent modified carbon quantum dots to sodium benzoate at various concentrations in test example 2 of the present invention;
FIG. 5 is a linear graph showing the effect of sodium benzoate at various concentrations on the fluorescence intensity of eutectic solvent modified carbon quantum dots in test example 2; wherein F is 0 Represents the initial fluorescence intensity of the carbon quantum dots, and F represents the fluorescence intensity after quenching by adding sodium benzoate solution.
Detailed Description
The present invention will be described in further detail with reference to the following examples in order to make the objects, technical solutions and advantages of the present invention more apparent. It should be understood that the specific embodiments described herein are for purposes of illustration only and are not intended to limit the scope of the invention.
Example 1
The preparation method of the eutectic solvent modified carbon quantum dot comprises the following steps:
a. crushing chestnut Pi Honggan, sieving with a 100-mesh sieve to obtain chestnut peel phenol, taking 0.1g of chestnut peel powder and 1g of glycolic acid/xylitol natural eutectic solvent (the preparation method of the glycolic acid/xylitol natural eutectic solvent comprises the steps of mixing glycolic acid and xylitol according to a molar ratio of 3:1, heating to 70-120 ℃ until a transparent uniform liquid is formed, mixing the liquid, namely the glycolic acid/xylitol natural eutectic solvent), adding 50mL of deionized water, stirring for 1h, uniformly mixing, centrifuging for 5min at 12000r/min, separating supernatant, and filtering the supernatant with a 0.22 mu m microfiltration membrane to obtain clear liquid;
b. adding the clear solution into a reaction kettle, heating to 220 ℃ for hydrothermal reaction for 11 hours, naturally cooling and drying to obtain a reaction solution, centrifuging the reaction solution for 10 minutes at 12000r/min, taking out the supernatant, and filtering with a microfiltration membrane of 0.22 mu m to obtain a filtrate which is the eutectic solvent modified carbon quantum dot.
And (3) observing and analyzing the prepared eutectic solvent modified carbon quantum dots by using a TEM, wherein a TEM image of the obtained eutectic solvent modified carbon quantum dots is shown in figure 1, and the carbon quantum dots are spherical, have smaller particle sizes and are about 2-5nm.
The fluorescence spectrum of the prepared eutectic solvent modified carbon quantum dot is shown in figure 2, and the fluorescence intensity of the carbon quantum dot solution is maximum at the wavelength of 350 nm.
Example 2
The preparation method of the eutectic solvent modified carbon quantum dots is the same as in example 1, and the relevant parameters are changed as follows:
| chestnut skin | 0.1g |
| Glycolic acid/xylitol natural eutectic solvent | 0.8g |
| Deionized water | 45mL |
| Temperature and time of hydrothermal reaction | 200℃、10h |
Other parameters are the same as in example 1, and the eutectic solvent modified carbon quantum dot is prepared.
Example 3
The preparation method of the eutectic solvent modified carbon quantum dots is the same as in example 1, and the relevant parameters are changed as follows:
| chestnut skin | 0.1g |
| Glycolic acid/xylitol natural eutectic solvent | 1.2g |
| Deionized water | 55mL |
| Temperature and time of hydrothermal reaction | 220℃、10h |
Other parameters are the same as in example 1, and the eutectic solvent modified carbon quantum dot is prepared.
Comparative example 1
The chestnut shell in example 1 is replaced by melon seed shell, and other preparation methods and raw materials are the same as those in example 1, so as to obtain the eutectic solvent modified carbon quantum dot.
Comparative example 2
The chestnut skin in example 1 was replaced with the pomegranate rind, and other preparation methods and raw materials were the same as in example 1, to obtain eutectic solvent modified carbon quantum dots.
Comparative example 3
The chestnut skin in example 1 was replaced with a citrus peel, and other preparation methods and raw materials were the same as in example 1, to obtain eutectic solvent-modified carbon quantum dots.
Test example 1
The fluorescence intensities of the eutectic solvent modified carbon quantum dots obtained in example 1 and comparative examples 1 to 3 were compared, and the detection results are shown in fig. 3, wherein the fluorescence intensity of the eutectic solvent modified carbon quantum dots prepared in example 1 is significantly higher than that of the eutectic solvent modified carbon quantum dots prepared in comparative documents 1 to 3.
Test example 2
The detection experiment of sodium benzoate as food preservative was performed on the eutectic solvent modified carbon quantum dots prepared in example 1.
Sodium benzoate solutions at concentrations of 8mM, 4mM, 1mM and 40. Mu.M were prepared, 2mL of sodium benzoate solution at the above-mentioned different concentrations was added to the prepared 2mL of carbon quantum dot solution at room temperature, and the change in fluorescence intensity of the carbon quantum dot was recorded. The results are shown in fig. 4, wherein the fluorescence intensity of the carbon quantum dot solution is lower as the concentration of the sodium benzoate solution is increased. Illustrative the eutectic solvent modified carbon quantum dots prepared in example 1 can be used to detect sodium benzoate as a preservative.
The fluorescence intensity of the carbon quantum dots prepared in example 1 was decreased with the increase of the concentration of sodium benzoate solution, i.e. the change of the fluorescence intensity of the carbon quantum dots and the concentration of sodium benzoate followed a certain linear rule, which indicates that the prepared carbon quantum dots can be used to detect the concentration of sodium benzoate in sodium benzoate solution. And through detection and calculation, the detection limit of the carbon quantum dot probe on sodium benzoate is 0.7mM, the linear regression equation is y=0.026x+0.203, and R is as follows 2 = 0.9935, the linear curve of which is shown in fig. 5.
The fluorescence intensity of the carbon quantum dot fluorescent probes obtained in the examples 2 and 3, the quenching response of sodium benzoate and the detection limit of sodium benzoate are all detected and analyzed by the same detection and analysis method, the detection results of the quenching response of the fluorescence intensity of the sodium benzoate are basically equivalent to the detection results of the carbon quantum dots in the example 1, and the detection limit of sodium benzoate can reach 0.7mM.
The foregoing description of the preferred embodiments of the invention is not intended to be limiting, but rather is intended to cover all modifications, equivalents, or alternatives falling within the spirit and principles of the invention.
Claims (8)
1. A preparation method of a eutectic solvent modified carbon quantum dot is characterized by comprising the following steps: the method comprises the following steps:
a. mixing chestnut skin powder and a glycolic acid/xylitol natural eutectic solvent, adding deionized water, uniformly mixing, centrifuging and filtering to obtain clear liquid, wherein the preparation method of the glycolic acid/xylitol natural eutectic solvent comprises the following steps: mixing glycolic acid and xylitol according to a molar ratio of 2-4:1, and heating to 70-120 ℃ until transparent uniform liquid is formed, wherein the liquid is the natural eutectic solvent of the glycolic acid/the xylitol; the mass ratio of the chestnut skin powder to the glycolic acid/xylitol natural eutectic solvent is 1:8-12;
b. and heating the clear liquid to perform a hydrothermal reaction, and centrifuging and filtering after the hydrothermal reaction is completed to obtain a filtrate, wherein the filtrate is the eutectic solvent modified carbon quantum dots.
2. The method for preparing the eutectic solvent modified carbon quantum dots according to claim 1, wherein the method comprises the following steps: in the step a, the particle size of the chestnut skin powder is less than or equal to 0.15mm.
3. The method for preparing the eutectic solvent modified carbon quantum dots according to claim 1, wherein the method comprises the following steps: in the step a, the mass volume ratio of the chestnut skin powder to the deionized water is 1g:450-550mL.
4. The method for preparing the eutectic solvent modified carbon quantum dots according to claim 1, wherein the method comprises the following steps: in the step b, the temperature of the hydrothermal reaction is 200-220 ℃ and the time is 10-11 h.
5. The method for preparing the eutectic solvent modified carbon quantum dots according to claim 1, wherein the method comprises the following steps: in step a and step b, the filter membrane for filtration was a microfiltration membrane of 0.22 μm.
6. The eutectic solvent modified carbon quantum dot manufactured by the method for manufacturing the eutectic solvent modified carbon quantum dot of any one of claims 1 to 5.
7. The use of the eutectic solvent modified carbon quantum dot according to claim 6 for detecting sodium benzoate.
8. The use of the eutectic solvent modified carbon quantum dot according to claim 6 as a fluorescent detection probe for sodium benzoate.
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| CN113607709A (en) * | 2021-08-10 | 2021-11-05 | 河北科技大学 | Application of fluorescent carbon quantum dots in naphthenic acid detection and naphthenic acid detection method |
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| AU2020103861A4 (en) * | 2020-05-19 | 2021-02-18 | Sichuan Agricultural University | Preparation of chicken feather nitrogen-doped carbon quantum dots based fluorescent probes and paraquat detection method |
| CN112816465A (en) * | 2021-01-06 | 2021-05-18 | 武汉轻工大学 | Method for rapidly determining content of sodium benzoate in food |
| CN113607709A (en) * | 2021-08-10 | 2021-11-05 | 河北科技大学 | Application of fluorescent carbon quantum dots in naphthenic acid detection and naphthenic acid detection method |
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