CN116836699B - Carbon quantum dot based on shaddock peel and preparation method and application thereof - Google Patents

Carbon quantum dot based on shaddock peel and preparation method and application thereof Download PDF

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CN116836699B
CN116836699B CN202310451359.XA CN202310451359A CN116836699B CN 116836699 B CN116836699 B CN 116836699B CN 202310451359 A CN202310451359 A CN 202310451359A CN 116836699 B CN116836699 B CN 116836699B
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shaddock peel
carbon quantum
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CN116836699A (en
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姜秀娟
马袁
周游
肖茸丹
孟祎杰
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Sichuan University of Science and Engineering
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    • C01B32/00—Carbon; Compounds thereof
    • C01B32/15—Nano-sized carbon materials
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • 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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    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • 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"
    • G01N21/643—Measuring fluorescence of fluorescent products of reactions or of fluorochrome labelled reactive substances, e.g. measuring quenching effects, using measuring "optrodes" non-biological material
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    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2002/00—Crystal-structural characteristics
    • C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
    • C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
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    • 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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    • 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"
    • G01N2021/6443—Fluorimetric titration

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Abstract

The invention discloses a carbon quantum dot based on shaddock peel and a preparation method and application thereof. The carbon quantum dot is prepared by mixing pretreated shaddock peel powder and L-tyrosine in a mass ratio of 1:1 and utilizing hydrothermal synthesis, has a fluorescence lifetime of higher than 3.5ns and a fluorescence quantum yield of higher than 0.2, has high sensitivity to synthetic pigment lemon Huang Shibie in food and selectivity specificity, and is very suitable for measuring lemon yellow in food such as beverage, candy and the like.

Description

Carbon quantum dot based on shaddock peel and preparation method and application thereof
Technical Field
The invention belongs to the field of food detection, and particularly relates to a carbon quantum dot based on shaddock peel, and a preparation method and application thereof.
Background
Natural pigments have been gradually replaced by synthetic pigments due to their active nature, high cost, sensitivity to light, heat and acid-base, however, the allowable addition amount of synthetic pigments has been increasingly reduced in consideration of consumer health. But are still widely used worldwide due to the price advantage of synthetic pigments. However, in recent years, with the occurrence of a series of events such as toxic cans and colored steamed bread, food safety has become the center of life, and the national standard GB 5009-2016 describes in detail the types of synthetic pigments and natural pigments that are allowed to be added and the maximum allowable amounts in different foods. Therefore, the detection method with low cost, simplicity, rapidness and high sensitivity is established and has important practical significance for supervision and management of food safety.
Carbon Quantum Dots (CQDs) are widely focused as a novel fluorescent nano material, and have the advantages of low cost, simple preparation, high fluorescence intensity, good chemical stability, easy functionalization and the like. Compared with semiconductor quantum dots and organic dyes, CQDs are green materials with good water solubility, good light stability, low toxicity and good biocompatibility. These properties make CQDs have broad application prospects in the fields of food analysis, biological imaging, biomolecule/drug delivery and the like. Therefore, the screening of CQDs with high sensitivity and good selectivity for identifying certain synthetic pigments in foods plays an important role in detecting edible synthetic pigments.
Disclosure of Invention
The invention aims to provide a carbon quantum dot based on shaddock peel, a preparation method and application thereof.
In order to achieve the aim of the invention, the invention is realized by adopting the following technical scheme:
the invention provides a preparation method of carbon quantum dots based on shaddock peel, which comprises the following steps:
(1) Drying and crushing the shaddock peel to obtain shaddock peel powder;
(2) Mixing the shaddock peel powder with amino acid, cooling to room temperature after high-temperature reaction, and obtaining the carbon quantum dots after dilution, filtration and purification.
Further, the amino acid is L-tyrosine.
Further, the mass ratio of the shaddock peel powder to the amino acid is 1:1.
Further, the high-temperature heating temperature is 200 ℃, and the heating time is 6 hours.
Further, the filtration was performed using a 0.22 μm microporous filter membrane.
The invention also provides the shaddock peel carbon quantum dot prepared by the preparation method, which has the fluorescence lifetime higher than 3.5ns and the fluorescence quantum yield higher than 0.2.
The invention also provides application of the shaddock peel carbon quantum dot in detecting food synthetic pigment.
Further, the food synthesis color is lemon yellow.
Furthermore, the shaddock peel carbon quantum dot has detection specificity on lemon yellow.
Furthermore, the detection limit of the shaddock peel carbon quantum dot is 0.0214mg/g.
Compared with the prior art, the invention has the following advantages and beneficial effects:
1. according to the invention, the natural shaddock peel is taken as a basic raw material, and is modified by doping N element, so that the identification performance and the luminous performance of the natural shaddock peel are improved, and the shaddock peel carbon quantum dot with better water solubility is prepared by a hydrothermal synthesis method. Experiments prove that the carbon quantum dots of the shaddock peel have high sensitivity to the synthetic pigment lemon Huang Shibie in food, have detection specificity, and do not cause any interference to the identification of lemon yellow by other coexists.
2. The detection limit of the carbon quantum dots of the shaddock peel is as follows: 4.36×10 -5 mol/L, namely: 0.0214mg/g, which is lower than the national standard of 0.1mg/g, so that the method is very suitable for measuring the lemon yellow in foods such as beverages, candies and the like.
Drawings
FIG. 1 is a structural characterization result of N-CQDs;
FIG. 2 is an XPS energy spectrum of N-CQDs;
FIG. 3 is a FT-IR spectrum of N-CQDs;
FIG. 4 is an XRD pattern for N-CQDs;
FIG. 5 is a graph of the ultraviolet absorption spectrum of N-CQDs;
FIG. 6 is a graph of recognition performance test results of N-CQDs;
FIG. 7 is a graph of interference test results for N-CQDs;
FIG. 8 is a graph of fluorescence titration results for N-CQDs;
FIG. 9 is a graph of fluorescence lifetime results for N-CQDs;
FIG. 10 is a chart showing the measurement of the lemon yellow pigment content of N-CQDs.
Detailed Description
The technical scheme of the invention is further described in detail by combining the following specific examples.
In the following examples, unless otherwise specified, all experimental methods used are conventional and all materials, reagents, etc. are commercially available from biological or chemical reagent companies.
Example 1: preparation of novel N-CQDs
Pretreatment of shaddock peel: drying pericarpium Citri Grandis, pulverizing, sieving, and weighing.
Mixing 300mg of pretreated shaddock peel powder with 300mg of L-tyrosine, pouring the mixture into a high-pressure reaction kettle, adding 10mL of ultrapure water, reacting for 6 hours at 200 ℃, naturally cooling to room temperature after the reaction is finished, diluting the obtained product, filtering and purifying the product by using a microporous filter membrane with the thickness of 0.22 mu m to obtain a final product N-CQDs, and collecting the final product and storing the final product at the temperature of 4 ℃ for later use.
Example 2: characterization and Performance Studies of novel N-CQDs
1. Characterization of novel N-CQDs
The N-CQDs prepared in example 1 were subjected to morphology, structure and particle size analysis, and structural characterization was performed by TEM, XRD spectroscopy, etc.; the elements and surface functional groups of N-CQDs are mainly characterized by XPS energy spectrum, FT-IR spectrum and the like.
The results of TEM and particle size of N-CQDs are shown in FIG. 1, and it can be seen that the morphology of the carbon dots is uniform, the morphology is relatively regular, no obvious aggregation is caused in the aqueous solution, the distribution is relatively uniform, and the particle size is about 5 nm.
XPS spectra and FT-IR spectra (FIGS. 2a-2d and 3) show that the main functional groups of N-CQDs are: amides, aromatic hydrocarbons, carboxylic acids, phenols, ketones, and the like.
The XRD spectrum (FIG. 4) shows that XRD has a broad diffraction peak at 22℃due to the amorphous structure of N-CQDs.
The results in FIG. 5 show that N-CQDs UV absorption is substantially consistent with tyrosine, demonstrating that doped tyrosine plays an important role in CQDs recognition performance.
2. Research on recognition performance of novel N-CQDs on synthetic pigment
(1) Selectivity study
1mL of amaranth, carmine, erythrosine, neored, allura red, lemon yellow, sunset yellow, brilliant blue, indigo, beta-carotene, sodium copper chlorophyll, titanium dioxide and other synthetic pigments with the concentration of 1mg/mL are respectively added into 2mL of carbon dot solution with the concentration of 0.2ug/mL, and the changes of the synthetic pigments are detected to determine whether the synthetic pigments have the performance of identifying the synthetic pigments.
The fluorescence spectrometer and the ultraviolet-visible spectrometer are respectively used for carrying out spectrum analysis on the N-CQDs, and the N-CQDs with good identification performance are screened out.
The results are shown in FIG. 6, where N-CQDs are only for lemon Huang Cumie, indicating that the carbon dot has a single selectivity.
(2) Interference test
Exploring the effect of common coexisting materials in beverages on recognition of pigments, adding to solutions containing carbon dots-lemon yellow, respectively: d-isoascorbic acid, sodium chloride, potassium sulfate, glycine, disodium hydrogen phosphate (dodecanol), sucrose, vanillin, magnesium chloride, sodium acetate, barium chloride, potassium nitrate, rose essence powder, sodium cyclamate, aluminum trichloride (hexahydrate), compound amino acid, urea, potassium chloride, ferrous sulfate, lemon yellow, sucralose, anhydrous glucose, L-cysteine, anhydrous calcium chloride, reduced glutathione, sunset yellow, copper acetate, zinc chloride and the like.
The results are shown in FIG. 7, which shows that the coexisting materials do not interfere with the identification of lemon yellow.
(3) Fluorescence titration
To further investigate the recognition of lemon yellow by N-CQDs, fluorescence titration was performed.
As a result, as shown in FIG. 8, fluorescence was gradually quenched with the gradual addition of lemon yellow. Limit of detection: 4.36×10 - 5 mol/L, namely: 0.0214mg/g, which is lower than the national standard of 0.1mg/g, so that the N-CQDs can be used for measuring the lemon yellow in beverages, candies and other foods.
3. Determination of fluorescence quantum yield of carbon quantum dots
The fluorescence quantum yields of N-CQDs were determined using the quinine sulfate reference method. The calculation formula is as follows:
Qc＝Qs*Fc/Fs*As/Ac*R 2 c/R 2 s
q represents the fluorescence quantum yield (qs=0.56); f represents the integral area of the corresponding fluorescence spectrogram; a represents ultraviolet absorbance; r represents the refractive index of the solvent. (c represents CQDs, s represents quinine sulfate)
As a result, as shown in FIG. 9, the fluorescence lifetime was 3.94ns; N-CQDs fluorescence quantum yield: 0.2780.
example 3: potential application of novel N-CQDs in food detection
When the constructed N-CQDs are used for analysis and detection of synthetic pigments, the performances of selectivity, stability, detection limit, reproducibility and the like of the synthetic pigments are to be examined. CQDs with quick response, good selectivity and high sensitivity are used for detecting synthetic pigments in foods such as beverages, candies and the like.
Referring to the literature, a standard curve is drawn with lemon yellow concentration as abscissa and fluorescence intensity as ordinate, and the equation is y= -3346.9x+836.83 (R 2 = 0.9938), the lemon yellow content in the jiale beverage was determined. And 3mL of the beverage is taken, and different doses of carbon point mother liquor are added into the beverage, wherein the carbon point concentration is 0.05ug/L, so that the beverage can effectively quench lemon yellow.
TABLE 1 preparation of standard curves
The standard curve was used to calculate the lemon Huang Midu ρ (mg/ml) in the beverage and the lemon yellow content in a beverage was measured to be about 0.0607mg/g in combination with the formula ω=3ρ/m (mg/g). Then, 0.19mL (0.0622 mg/g) of lemon yellow standard solution was added to the beverage for labeling recovery, and the recovery rate was 86.82%.
The above embodiments are only for illustrating the technical solution of the present invention, and are not limiting; although the invention has been described in detail with reference to the foregoing embodiments, it will be apparent to one skilled in the art that modifications may be made to the technical solutions described in the foregoing embodiments, or equivalents may be substituted for some of the technical features thereof; such modifications and substitutions do not depart from the spirit and scope of the corresponding technical solutions.

Claims (6)

1. The preparation method of the carbon quantum dot based on the shaddock peel is characterized by comprising the following steps of:
(1) Drying and crushing the shaddock peel to obtain shaddock peel powder;
(2) Mixing the shaddock peel powder with amino acid, pouring the mixture into a high-pressure reaction kettle, adding ultrapure water, cooling to room temperature after high-temperature reaction, and obtaining carbon quantum dots after dilution and purification; the amino acid is L-tyrosine; the temperature of the high-temperature reaction is 200-220 ℃, and the heating time is 6-8 hours.
2. The preparation method of claim 1, wherein the mass ratio of the shaddock peel powder to the amino acid is 1:1-3.
3. The shaddock peel carbon quantum dot prepared by the preparation method of any one of claims 1-2, wherein the fluorescent lifetime of the shaddock peel carbon quantum dot is higher than 3.5ns, and the fluorescent quantum yield is higher than 0.2.
4. The application of the shaddock peel carbon quantum dot in detecting food synthetic pigment according to claim 3, wherein the food synthetic pigment is lemon yellow.
5. The use according to claim 4, wherein the shaddock peel carbon quantum dot has detection specificity for lemon yellow.
6. The use according to claim 4, wherein the detection limit of the shaddock peel carbon quantum dot is 0.0214mg/g.
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Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105001862A (en) * 2015-07-30 2015-10-28 西华师范大学 Preparation of carbon quantum dots by use of aloe as carbon source and detection method of lemon yellow
CN105802621A (en) * 2016-04-05 2016-07-27 南京理工大学 N-CQDs (nitrogen-doped carbon quantum dots) with high fluorescence quantum yield as well as preparation method and application of N-CQDs
CN108489951A (en) * 2018-04-20 2018-09-04 吉林大学 Double fluorescent emission copper nano-cluster/carbon dots colorimetric probes, preparation method and the application in trace water context of detection
CN109490269A (en) * 2018-12-07 2019-03-19 吉林大学 The application of double transmitting colorimetric fluorescent nanometer microsphere preparation methods and its Bacteria Detection
CN109504373A (en) * 2018-11-29 2019-03-22 山西大学 A kind of chlorine nitrogen codope carbon quantum dot and its preparation method and application based on the preparation of discarded pomelo peel
CN113201336A (en) * 2021-05-19 2021-08-03 扬州大学 Preparation method based on nitrogen-phosphorus doped carbon quantum dots and application of preparation method in rapid detection of tartrazine
CN113943573A (en) * 2021-11-12 2022-01-18 成都理工大学 Method for preparing fluorescent carbon quantum dots and detecting tartrazine by aid of alligator alternanthera

Patent Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105001862A (en) * 2015-07-30 2015-10-28 西华师范大学 Preparation of carbon quantum dots by use of aloe as carbon source and detection method of lemon yellow
CN105802621A (en) * 2016-04-05 2016-07-27 南京理工大学 N-CQDs (nitrogen-doped carbon quantum dots) with high fluorescence quantum yield as well as preparation method and application of N-CQDs
CN108489951A (en) * 2018-04-20 2018-09-04 吉林大学 Double fluorescent emission copper nano-cluster/carbon dots colorimetric probes, preparation method and the application in trace water context of detection
CN109504373A (en) * 2018-11-29 2019-03-22 山西大学 A kind of chlorine nitrogen codope carbon quantum dot and its preparation method and application based on the preparation of discarded pomelo peel
CN109490269A (en) * 2018-12-07 2019-03-19 吉林大学 The application of double transmitting colorimetric fluorescent nanometer microsphere preparation methods and its Bacteria Detection
CN113201336A (en) * 2021-05-19 2021-08-03 扬州大学 Preparation method based on nitrogen-phosphorus doped carbon quantum dots and application of preparation method in rapid detection of tartrazine
CN113943573A (en) * 2021-11-12 2022-01-18 成都理工大学 Method for preparing fluorescent carbon quantum dots and detecting tartrazine by aid of alligator alternanthera

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