CN106978160A - Nitrogen sulfur doping carbon namo fluorescence probe environment-friendly preparation method thereof - Google Patents
Nitrogen sulfur doping carbon namo fluorescence probe environment-friendly preparation method thereof Download PDFInfo
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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
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Abstract
The invention discloses a kind of nitrogen sulfur doping carbon namo fluorescence probe environment-friendly preparation method thereof, comprise the following steps：A, using the fish processing waste rich in protein as raw material, it is 10 100 grams of flesh of fish block that quality is cut into after cleaning；B, the flesh of fish block raw material after stripping and slicing is heat-treated, wherein heat treatment temperature is 100 500 DEG C, and processing time is 10 60 min；C, by the flesh of fish block Jing Guo baking be soaked in organic solvent extract, wherein extraction time be 2 48 hours, solid-liquid ratio is 1:1‑1:10；After D, extraction processing, liquid phase is collected, rotary evaporation removes organic solvent；Purified after E, fat-soluble organic solvent degreasing using volume exclusion gel filtration chromatography, with being carbon namo fluorescence probe after being compounded containing ferric ion compounds, wherein nano particle and iron ion mass ratio are 20:1‑5:1.Nitrogen sulfur doping carbon namo fluorescence probe environment-friendly preparation method thereof of the present invention, detection process is simple to operate, sensitivity is high and selectivity is good, and testing result is directly perceived, can quantify and detect.
Description
Technical field
The present invention relates to the preparation of fluorescence probe and applied technical field, more particularly to a kind of nitrogen sulfur doping carbon nano fluorescent
Probe environment-friendly preparation method thereof.
Background technology
In the prior art, carbon nano-particle refers to that diameter is less than 100 nanometers of particle, and carbon nano-particle has excellent light
Performance is learned, bright fluorescence can be sent in the presence of specific wavelength exciting light, in metal ion detection, bio-imaging, medicine
The fields such as thing delivering are had a wide range of applications, for its preparation method, including top-down cracked by bulk matter is made
Method for nano particle and the method for polymerizeing synthesis nano particle by small molecule from bottom to top, top-to-bottom method lead to
More exacting terms is often needed, and the nano-particle fluorescence yield prepared is relatively low, preparation method letter from bottom to top
It is single, in that context it may be convenient to prepare nano particle, generally by using the method for doping other elements, obtain high-fluorescence quantum yield
Carbon nano-particle, it is nitrogen to be usually used in doped chemical, on the other hand, and the recycling of discarded object is also very important in Green Chemistry
Problem, the method for preparing nitrogen sulfur doping carbon point by fish processing waste at present has not been reported, vitamin C be it is a kind of oneself
Sugared formylsalicylic acid, with antiscorbutic effect, also referred to as ascorbic acid, important work is played in terms of health is maintained
With, meanwhile, vitamin C or a kind of antioxidant and free radical scavenger can relax the oxidative stress of a variety of diseases, be one
The organic compound closely related with vital movement is planted, vitamin C is a kind of water soluble vitamin, unstable under normal conditions, held
Easily aoxidized, easily influenceed by temperature, pH value, enzyme, copper ion, iron ion, ultraviolet and sugar, salt etc. by the oxygen in air；
For the mankind, vitamin C must be absorbed from food, therefore, and detection Vitamin C content can not only evaluate food
Product quality, also to research vitamin C, all tool is of great significance in terms of healthy diet, health care and food fresh keeping.
The content of the invention
Traditional preparation method is broken through it is an object of the invention to provide one kind, reduction production cost is low, implementation process is simple, can
The nitrogen sulfur doping carbon namo fluorescence probe environment-friendly preparation method thereof of control.
The technical scheme that is used to achieve the above object of the present invention is：A kind of nitrogen sulfur doping carbon namo fluorescence probe green
Preparation method, comprises the following steps：
A, using the fish processing waste rich in protein as raw material, it is 10-100 grams of flesh of fish block that quality is cut into after cleaning；
B, the flesh of fish block raw material after stripping and slicing is heat-treated, wherein heat treatment temperature is 100-500 DEG C, and processing time is 10-
60 min；
C, the flesh of fish block Jing Guo baking is soaked in organic solvent extracted, wherein extraction time is 2-48 hours, and solid-liquid ratio is
1:1-1:10；
After D, extraction processing, liquid phase is collected, rotary evaporation removes organic solvent；
After E, fat-soluble organic solvent degreasing using volume exclusion gel filtration chromatography purify, with compounded containing ferric ion compounds after i.e.
For carbon namo fluorescence probe, wherein nano particle and iron ion mass ratio are 20:1-5:1.
The step A Mesichthyes is freshwater fish.
The maximum gauge that block is oppressed in the step A is 0.1-10 centimetres.
Organic solvent in the step C is the one or more in ethanol, methanol, ether, ethyl acetate.
In the step E fat-soluble organic solvent be chloroform, dichloromethane, n-hexane, isopropanol in one kind or
It is several.
Volume exclusion gel column is one in cross-link dextran, Ago-Gel, polyacrylamide gel in the step E
Plant or several.
In the step E containing ferric ion compounds be iron chloride, ferric nitrate, ferric acetate, ferric sulfate molysite and they
Hydrate.
A kind of nitrogen sulfur doping carbon namo fluorescence probe environment-friendly preparation method thereof of the present invention, detection process is simple to operate, spirit
Sensitivity is high and selectivity is good, and testing result is directly perceived, can quantify and detect.
Brief description of the drawings
Fig. 1 is that a kind of carbon of the preparation of embodiment one of nitrogen sulfur doping carbon namo fluorescence probe environment-friendly preparation method thereof of the invention is received
The particle diameter distribution schematic diagram of rice fluorescence probe.
Fig. 2 is that a kind of carbon of the preparation of embodiment one of nitrogen sulfur doping carbon namo fluorescence probe environment-friendly preparation method thereof of the invention is received
The x-ray photoelectron energy-spectrum scanning figure of rice fluorescence probe.
Fig. 3 is that a kind of carbon of the preparation of embodiment one of nitrogen sulfur doping carbon namo fluorescence probe environment-friendly preparation method thereof of the invention is received
The fine spectrograms of C1s of rice fluorescence probe.
Fig. 4 is that a kind of carbon of the preparation of embodiment one of nitrogen sulfur doping carbon namo fluorescence probe environment-friendly preparation method thereof of the invention is received
The fine spectrograms of N1s of rice fluorescence probe.
Fig. 5 is that a kind of carbon of the preparation of embodiment one of nitrogen sulfur doping carbon namo fluorescence probe environment-friendly preparation method thereof of the invention is received
The fine spectrograms of O1s of rice fluorescence probe.
Fig. 6 is that a kind of carbon of the preparation of embodiment one of nitrogen sulfur doping carbon namo fluorescence probe environment-friendly preparation method thereof of the invention is received
The fine spectrograms of S2p of rice fluorescence probe.
Fig. 7 is that a kind of carbon of the preparation of embodiment one of nitrogen sulfur doping carbon namo fluorescence probe environment-friendly preparation method thereof of the invention is received
The infrared spectrogram of rice fluorescence probe.
Fig. 8 is the Fe in a kind of embodiment two of nitrogen sulfur doping carbon namo fluorescence probe environment-friendly preparation method thereof of the invention3+It is dense
Spend the influence schematic diagram to fluorescence intensity.
Fig. 9 is the vitamin in a kind of embodiment five of nitrogen sulfur doping carbon namo fluorescence probe environment-friendly preparation method thereof of the invention
Influence schematic diagram of the C concentration to fluorescence intensity.
Embodiment
As shown in Fig. 1-Fig. 9, nitrogen sulfur doping carbon namo fluorescence probe environment-friendly preparation method thereof comprises the following steps：
A, using the fish processing waste rich in protein as raw material, it is 10-100 grams of flesh of fish block that quality is cut into after cleaning,
Wherein maximum gauge is 0.1-10 centimetres, and its Mesichthyes is the freshwater fishes such as crucian, carp；B, by the flesh of fish block raw material after stripping and slicing
It is heat-treated, wherein heat treatment temperature is 100-500 DEG C, processing time is 10-60 min；C, by the flesh of fish block Jing Guo baking
It is soaked in organic solvent and extracts, wherein extraction time is 2-48 hours, and solid-liquid ratio is 1:1-1:10, organic solvent includes second
One or more in alcohol, methanol, ether, ethyl acetate,；After D, extraction processing, liquid phase is collected, rotary evaporation removes organic molten
Agent；After E, fat-soluble organic solvent degreasing using volume exclusion gel filtration chromatography purify, with compounded containing ferric ion compounds after i.e.
For carbon namo fluorescence probe, wherein nano particle and iron ion mass ratio are 20:1-5:1, there is fat-soluble organic solvent to include three
One or more in chloromethanes, dichloromethane, n-hexane, isopropanol, volume exclusion gel column includes：Sephadex is crosslinked
One or more in glucan, Sepharose Ago-Gels, Bio-Gel P polyacrylamide gels, iron content ionization
Compound includes：The molysite such as iron chloride, ferric nitrate, ferric acetate, ferric sulfate and their hydrate, the carbon namo fluorescence probe should
For reducing substances detection, especially ascorbic detection, it is 250-400 nanometers that optical range is excited in detection, launches light model
It is 400-600 nanometers to enclose, and ascorbic detection is based on the transmitting of " On-Off-On " tri-state.
Embodiment one：The preparation of the carbon nano-particle of nitrogen sulfur doping, crucian is cleaned, and 10-20 g cube meat is cut into, 400
Nano particle is extracted by alcohol steep after DEG C min of baking 30, natural cooling, solid-liquid ratio is 1:5, extraction time is 15 hours；
The ethanol in alcohol extracts is removed by vacuum rotary evaporator；Residue uses chloroform extraction after being redissolved using water
The volume ratio of degreasing, water and chloroform is 1:1, untill aqueous phase solution clear（It is repeated 5 times）；Aqueous phase is slightly carried into solution
G-25 sephadex column chromatographies are crossed, fluorescence intensity is collected and is higher than 80（The nm of excitation wavelength=340, the nm of launch wavelength=410）Portion
Point, the powdered carbon nano-particle obtained after freezing by transmission electron microscope observing, it is found that its is spherical in shape, average grain diameter is
16.7 nm, carbon nano fluorescent yield is measured by known formula, Φ 1=Φ 2I1A2 η 21/I2A1 η 22, it is desirable to absorbance
A1, A2 are less than 0.1, and to reduce error, reference substance, the integral area of I2- quinine sulfate fluorescence intensities are used as using quinine sulfate
Value, the integrated area value of I1- nano-particle fluorescence intensity, the ultraviolet absorption value of A2- quinine sulfates, A1- nano-particle fluorescences are strong
The ultraviolet absorption value of degree, the refractive index of η 2- quinine sulfate solvents, the refractive index of η 1- nano particles.Prepare carbon Nano quantum fluorescence
Quantum yield is 12.6%, by X-ray photoelectron spectroscopic analysis, and obtained nano particle is made up of carbon, nitrogen, oxygen and sulphur, and it compares
Example is 57.15%, 15.64%, 26.1% and 1.11%, meanwhile, X-ray photoelectron spectroscopic analysis and FTIR spectrum analytical table
Contain abundant functional group, including hydroxyl, carbonyl, amino etc. in its bright surface.
Embodiment two：The preparation of the carbon namo fluorescence probe detected for vitamin C, by obtained nanometer in embodiment one
Particle is configured to the aqueous solution that concentration is 0.1 mg mL-1, and iron chloride is added thereto, its final concentration is distinguished 10,20,
40,60,80,100,150,300,400,500 μm of ol L-1, it is rear to stand 2 min after being sufficiently mixed, using detection
Wave-length coverage covers the fluorescence intensity F1 in 280-700nm fluophotometer examination criteria solution, and testing conditions are excitation wave
A length of 340 nm, the nm of launch wavelength 410, blank control group（Not plus iron ion）Fluorescence intensity be F0（Excitation wavelength is
340 nm, the nm of launch wavelength 410）, draw out fluorescent quenching intensity（（F0- F1）/ F0）With the standard between Fe3+ concentration
Curve, Fig. 8 is sensitivity analysis figure of the carbon namo fluorescence probe to Fe3+, it is seen that with the increase of Fe3+ concentration, carbon nanometer
Grain fluorescence intensity is gradually reduced, and illustrates that the carbon nano-particle is very sensitive to Fe3+ concentration；But as [Fe3+] >=100 μm ol
During L-1, the reduction of the fluorescence intensity of carbon nano-particle and the rise of iron concentration no longer have linear relationship；It is molten with Fe3+
Liquid concentration range is abscissa in 10-100 μm of ol L-1, with fluorescent quenching intensity（（F0- F1）/ F0）, can for ordinate
Equation of linear regression y=0.00378x+0.01998, coefficient R 2=0.9948 is made, by nanometer made from 1 in embodiment
Grain is configured to the aqueous solution that concentration is 0.1 mg mL-1, adds ferric chloride solution, is allowed to final concentration of 40 μm of ol L-1, stands
After 10 minutes, nano particle can obtain fluorescence probe after coordinating with iron ion, under 340 nanometers of exciting lights, at 410 nanometers
Lower fluorescence intensity, its fluorescence intensity is quenched because of the presence of iron ion, can be used for ascorbic detection.
Embodiment three：The preparation of the carbon namo fluorescence probe detected for vitamin C, by obtained nanometer in embodiment one
Particle is configured to the aqueous solution that concentration is 0.1 mg mL-1, adds ferric chloride solution, is allowed to final concentration of 100 μm of ol L-1,
After standing 10 minutes, nano particle can obtain fluorescence probe after coordinating with iron ion, under 340 nanometers of exciting lights, 410
The lower fluorescence intensity of nanometer, can be used for ascorbic detection.
Example IV：The preparation of the carbon namo fluorescence probe detected for vitamin C, by obtained nanometer in embodiment one
Particle is configured to the aqueous solution that concentration is 0.1 mg mL-1, adds ferric chloride solution, is allowed to final concentration of 150 μm of ol L-1.It is quiet
Put after 10 minutes, nano particle can obtain fluorescence probe after coordinating with iron ion.Under 340 nanometers of exciting lights, received 410
The lower fluorescence intensity of rice, can be used for ascorbic detection.
Embodiment five：Ascorbic detection, obtained carbon namo fluorescence probe in embodiment three is used to detect vitamin
C content, takes the above-mentioned carbon namo fluorescence probe solution of 1.9 mL, and adding vitamin C makes its final concentration be respectively 10,40,80,
150,250,400,500 μm of ol L-1, it is rear to stand 30 min after being sufficiently mixed, 280- is covered using Detection wavelength scope
Fluorescence intensity F1 in 700nm fluophotometer examination criteria solution, testing conditions are that excitation wavelength is 340 nm, transmitted wave
Long 410 nm, blank control group（Not plus iron ion）Fluorescence intensity be F0（Excitation wavelength is 340 nm, launch wavelength 410
nm ）, draw out fluorescent quenching intensity（（F1- F0）/ F0）Standard curve between vitamin C concentration, Fig. 9 is carbon nanometer
Fluorescence probe is to ascorbic sensitivity analysis figure, it is seen that carbon namo fluorescence probe is with the increase of vitamin C concentration, fluorescence
Intensity gradually rises, and illustrates the carbon namo fluorescence probe to ascorbic concentration sensitive；But as the μ of vitamin C concentration >=250
During mol L-1, the rise of the fluorescence intensity of carbon nanometer and the rise of vitamin C concentration no longer have linear relationship；With vitamin
C concentration ranges are abscissa in 10-250 μm of ol L-1, with fluorescent quenching intensity（（F0- F1）/ F0）For ordinate, it can make
Equation of linear regression y=0.000862x+0.01505, coefficient R 2=0.9108 are obtained, by obtained carbon nanometer in embodiment three
Fluorescence probe is used to detect ascorbic content, takes the above-mentioned carbon namo fluorescence probe solution of 1.9 mL, adds 0.1 mL 0.8
Mmol L-1 vitamin c solution, under 340 nanometers of exciting lights, the fluorescence intensity under 410 nanometers is adding reproducibility
After material, iron ion is reduced into ferrous ion, obtains extensive to a certain extent because iron ion presence causes fluorescence intensity to be quenched
Multiple, its recovery extent is directly proportional to reducing substances addition, realizes the response of " On-Off-On " of fluorescence, reaches measure mesh
, in this example, it is 0.84 mmol L-1 to be calculated according to standard curve and obtain its concentration, and the rate of recovery is 105%.
Embodiment six：Ascorbic detection, obtained carbon namo fluorescence probe in embodiment three is used to detect vitamin
C content, takes the above-mentioned carbon namo fluorescence probe solution of 1.9 mL, adds the mmol L-1 of 0.1 mL 1.6 vitamin c solution,
Under 340 nanometers of exciting lights, the fluorescence intensity under 410 nanometers, after reducing substances is added, iron ion is reduced into
Ferrous ion, is restored to a certain extent because iron ion presence causes fluorescence intensity to be quenched, its recovery extent and reproducibility
Material addition is directly proportional, and realizes the response of " On-Off-On " of fluorescence, measure purpose is reached, in this example according to standard curve
It is 1.82 mmol L-1 to calculate and obtain its concentration, and the rate of recovery is 114%.
Embodiment 7：Ascorbic detection, obtained carbon namo fluorescence probe in embodiment three is used to detect vitamin C
Content, take the above-mentioned carbon namo fluorescence probe solution of 1.9 mL, add the mmol L-1 of 0.1 mL 5.0 vitamin c solution,
Under 340 nanometers of exciting lights, the fluorescence intensity under 410 nanometers, after reducing substances is added, iron ion is reduced into Asia
Iron ion, is restored to a certain extent because iron ion presence causes fluorescence intensity to be quenched, its recovery extent and reproducibility thing
Matter addition is directly proportional, and realizes the response of " On-Off-On " of fluorescence, reaches measure purpose, in this example, according to standard curve
It is 5.2 mmol L-1 to calculate and obtain its concentration, and the rate of recovery is 104%, nitrogen sulfur doping carbon namo fluorescence probe green system of the present invention
Preparation Method, raw material is easy to get, cost is low, process is simply controllable, i.e., grilled fish is carried out simple organic solvent extraction, revolving, extraction,
Gel chromatography, gained carbon nanometer is less than 20 nanometers of chondritic for diameter, with fluorescence lifetime length, quantum efficiency it is high,
As a result reproducible the characteristics of.
Claims (7)
1. a kind of nitrogen sulfur doping carbon namo fluorescence probe environment-friendly preparation method thereof, it is characterised in that comprise the following steps：
A, using the fish processing waste rich in protein as raw material, quality is cut into after cleaning for 10-100 grams
Oppress block；
B, the flesh of fish block raw material after stripping and slicing is heat-treated, wherein heat treatment temperature is 100-500 DEG C, processing
Time is 10-60 min；
C, by the flesh of fish block Jing Guo baking be soaked in organic solvent extract, wherein extraction time be 2-48 hours,
Solid-liquid ratio is 1:1-1:10；
After D, extraction processing, liquid phase is collected, rotary evaporation removes organic solvent；
After E, fat-soluble organic solvent degreasing using volume exclusion gel filtration chromatography purify, with compounded containing ferric ion compounds after i.e.
For carbon namo fluorescence probe, wherein nano particle and iron ion mass ratio are 20:1-5:1.
2. a kind of nitrogen sulfur doping carbon namo fluorescence probe environment-friendly preparation method thereof according to claim 1, it is characterised in that：Institute
Step A Mesichthyes is stated for freshwater fish.
3. a kind of nitrogen sulfur doping carbon namo fluorescence probe environment-friendly preparation method thereof according to claim 1, it is characterised in that：Institute
State and the maximum gauge of block is oppressed in step A for 0.1-10 centimetres.
4. a kind of nitrogen sulfur doping carbon namo fluorescence probe environment-friendly preparation method thereof according to claim 1, it is characterised in that：Institute
It is the one or more in ethanol, methanol, ether, ethyl acetate to state the organic solvent in step C.
5. a kind of nitrogen sulfur doping carbon namo fluorescence probe environment-friendly preparation method thereof according to claim 1, it is characterised in that：Institute
It is the one or more in chloroform, dichloromethane, n-hexane, isopropanol to state fat-soluble organic solvent in step E.
6. a kind of nitrogen sulfur doping carbon namo fluorescence probe environment-friendly preparation method thereof according to claim 1, it is characterised in that：Institute
It is the one or more in cross-link dextran, Ago-Gel, polyacrylamide gel to state volume exclusion gel column in step E.
7. a kind of nitrogen sulfur doping carbon namo fluorescence probe environment-friendly preparation method thereof according to claim 1, it is characterised in that：Institute
State in step E containing ferric ion compounds be iron chloride, ferric nitrate, ferric acetate, ferric sulfate molysite and their hydrate.
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| CN108169198A (en) * | 2017-12-28 | 2018-06-15 | 大连工业大学 | Utilize the method for fluorescent carbon quantum dot detection Determination of Glucose in Food |
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108059148A (en) * | 2017-12-28 | 2018-05-22 | 大连工业大学 | The preparation method of nano-particle with Scavenging ability |
| CN108084997A (en) * | 2017-12-28 | 2018-05-29 | 大连工业大学 | The preparation method of N doping fluorescent carbon quantum dots |
| CN108083256A (en) * | 2017-12-28 | 2018-05-29 | 大连工业大学 | The preparation method of high fluorescence property fluorescent carbon quantum dot and its in Cr（VI）Application in detection |
| CN108169198A (en) * | 2017-12-28 | 2018-06-15 | 大连工业大学 | Utilize the method for fluorescent carbon quantum dot detection Determination of Glucose in Food |
| CN108587617A (en) * | 2018-06-22 | 2018-09-28 | 大连工业大学 | The preparation method of carbon nano-particles in roasting Spanish mackerel |
| CN109283235A (en) * | 2018-11-13 | 2019-01-29 | 汕头大学 | One kind being based on NSCQDs/Bi2S3Optical electro-chemistry sensor and its preparation and application |
| CN109283235B (en) * | 2018-11-13 | 2020-11-27 | 汕头大学 | Based on NSCQDs/Bi2S3Photoelectrochemical sensor and preparation method thereof |
| CN109358128A (en) * | 2018-12-03 | 2019-02-19 | 南京大学 | A kind of organic nitrogen-organic carbon tandem online test method and device |
| CN109358128B (en) * | 2018-12-03 | 2024-04-09 | 南京大学 | Organic nitrogen-organic carbon serial on-line detection method and device |
| CN109852386A (en) * | 2019-01-08 | 2019-06-07 | 大连工业大学 | A method of extracting fluorescent carbon quantum dot from canned fish |
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