CN109852386A - A method of extracting fluorescent carbon quantum dot from canned fish - Google Patents
A method of extracting fluorescent carbon quantum dot from canned fish Download PDFInfo
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- CN109852386A CN109852386A CN201910015139.6A CN201910015139A CN109852386A CN 109852386 A CN109852386 A CN 109852386A CN 201910015139 A CN201910015139 A CN 201910015139A CN 109852386 A CN109852386 A CN 109852386A
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Abstract
The method that the invention discloses a kind of to extract fluorescent carbon quantum dot from canned fish, comprising the following steps: the degreasing of THz wave assisted extraction, the extraction of ultrasonic wave Assisted Ethanol, concentration, alcohol precipitation removal of impurities, evaporation and concentration, dialysis purification, centrifugation, the carbon quantum dot with photoluminescent property is lyophilized to obtain in raw material crushing.The present invention is compared with general extraction methods, and carbon quantum dot yield improves 15%, and fluorescence intensity improves 20% or more, does not use organic solvent, green, and environmental protection is conducive to the application of carbon dots；Gained carbon quantum dot purity is high is extracted, has good stability, biocompatibility at low concentrations, can be used for the carrier of biomaterial, there is cytotoxicity in higher concentrations, can be used for the treatment of tumour cell.Since the fluorescence intensity of carbon quantum dot can characterize processing intensity, by examining fluorescence strong and weak, to adjust processing technology, the control to food processing process is realized.
Description
Technical field
The present invention relates to endogenous Hazard factors in food processing to generate control field, in particular to one kind is from canned fish
The method for extracting fluorescent carbon quantum dot.
Background technique
Carbon quantum dot refers to that particle diameter is less than the novel carbon nanomaterial with fluorescent characteristic of 10nm, because its is glimmering
The features such as photosensitiveness, hypotoxicity, good biocompatibility, is widely used in biological detection, gene operating, bio-imaging and drug
The fields such as transmission.Between past more than ten year, the scientist of various countries has been developed for the side of various different synthesis carbon quantum dots
Method is used for above-mentioned field.
In recent years, had found carbon quantum dot in many food processings, such as roast beef, roast mutton, toast bread, caramel,
Coca-Cola, beer etc., and carbon quantum dot can be also generated in food processing in most common Maillard reaction, these quantum dots are all
There is preferable fluorescence, has preferable similar intermiscibility at low concentrations, can be freely accessible in cell；However, the carbon of high concentration
Quantum dot can cause the death of cell, have cytotoxicity.Also it has been reported that, the fluorescence in Maillard reaction can indicate beauty
Maillard reaction degree, it is possible to by measuring the intensity of its fluorescence, carry out adjusting process, prevent processing excessively, prevent from endangering because
The generation of son.
Canned fish is one of product that people often eat, and work in-process is usually using fried, seasoning, and then high temperature kills again
Maillard reaction occurs for the technique of bacterium, and closely similar with the technique of scientists preparation carbon quantum dot.In tinned food from
It has no it has been found that carbon nano-particles, study it and be applied.
Summary of the invention
The method that the purpose of the present invention is to provide a kind of to extract fluorescent carbon quantum dot from canned fish, using first degreasing
Method is conducive to subsequent carbon quantum dot preparation, and extracting method is simple and efficient, and yield is high and gained carbon quantum dot fluorescence is stronger,
There are good fluorescent stability, biocompatibility at low concentrations, can be used for the carrier of biomaterial, can use in higher concentrations
Make the potential source biomolecule material for the treatment of tumour.Fluorescence intensity can be applied simultaneously, characterize the degree of Maillard reaction, control can food
The technical process of product processing, reduces the generation of hazardous material.
To achieve the above object, the technical scheme adopted by the invention is that:
A method of fluorescent carbon quantum dot is extracted from canned fish, comprising the following steps: raw material crushes, THz wave assists
It extracts degreasing, the extraction of ultrasonic wave Assisted Ethanol, concentration, alcohol precipitation removal of impurities, evaporation and concentration, dialysis purification, centrifugation, be lyophilized with glimmering
The carbon quantum dot of light property.
A method of extracting fluorescent carbon quantum dot from canned fish, comprising steps of
S1, raw material crush: the flesh of fish in canned fish is ground into fritter；
S2, THz wave assisted extraction degreasing:
It is primary to extract: by flesh of fish fritter obtained in step S1 according to solid-liquid ratio 1:(1~5) g/ml addition pure water, one
10~30min of secondary stirring, THz wave processing is carried out while the primary stirring, and filtering obtains the flesh of fish 1 and filtrate 1；
Second extraction: the flesh of fish 1 is according to solid-liquid ratio 1:(1~5) g/ml addition pure water, secondary agitation 10~30min of extraction,
THz wave processing is carried out while the secondary agitation, filtering obtains the flesh of fish and filtrate 2；Merge the filtrate 1 and filtrate 2, obtains
Filtrate；
S3, filtrate obtained by step S2 is centrifuged, removes grease, obtains aqueous extract；
S4, the extraction of ultrasonic wave Assisted Ethanol: by the gained flesh of fish in step S2 according to solid-liquid ratio 1:(1~3) g/ml, matter is added
The ethyl alcohol that score is 60%~100% to be measured, while utilizing Ultrasonic Wave-Assisted Extraction, the ultrasonic frequency is 20~80Hz, when
Between be 0.5~3h；It filters, takes filtrate；
S5, concentration: gained filtrate in the aqueous extract and step S4 in step S3 is merged, the 1/ of original volume is concentrated into
15~1/25, obtain concentrate；
S6, alcohol precipitation removal of impurities: by concentrate obtained in step S5 be added its 3~6 times of volumes mass fraction be 80%~
95% ethyl alcohol, at 4~15 DEG C, stand 10~for 24 hours；Centrifuging and taking supernatant；
S7, evaporation and concentration: gained supernatant in step S6 is concentrated into the 1/6~1/10 of original volume, obtained through pervaporation
Concentrate；
S8, dialysis purification: dialysing to the resulting concentrate of step S7 using deionized water, the solution after taking dialysis；
S9, centrifugation: by the solution centrifuging and taking supernatant after gained dialysis in step S8；
S10, freeze-drying: by gained supernatant in step S9, freeze-drying obtains the carbon quantum dot with photoluminescent property.
Preferably, fritter described in step S1 specifically: 0.5cm × 0.5cm × 0.5cm~2cm × 2cm × 2cm；The fish
Can is one of chrysanthemum canned fish, dace with black bean can, roast eel canned fish, phoenix tail canned fish；The canned fish is preferably
The canned fish made by frying technological process.
Preferably, the frequency of THz wave described in step S2 is 0.18~0.3THz, and power is 20~40KW.
Preferably, it is centrifuged described in step S3 are as follows: 4 DEG C, 8000r/min are centrifuged 10min.
Preferably, concentration described in step S5 is vacuum concentration, design parameter are as follows: 40~60 DEG C, vacuum degree -0.08~-
0.1MPa。
Preferably, it is centrifuged described in step S6 are as follows: 4 DEG C, 8000r/min are centrifuged 10min.
Preferably, rotary evaporation, design parameter are evaporated to described in step S7 are as follows: 50~70 DEG C of rotating evaporation temperature, revolving speed
For 30~60r/min, vacuum degree -0.08~-0.1MPa.
Preferably, step S8 specifically: concentrate obtained by step S7 is placed in the bag filter with 1KDa molecular weight, is used
The deionized water of 5~15 times of volumes dialyses to it, and every 4h changes a deionized water, changes water 3~5 times.
Preferably, it is centrifuged described in step S9 are as follows: 8000r/min is centrifuged 10min.
Preferably, it is freeze-dried described in step S10 specifically: shelf temperature -45~60 DEG C, vacuum degree≤5Pa, when dry
Between 12~for 24 hours.
Beneficial effects of the present invention are as follows:
1, for the present invention compared with other preparation carbon quantum dot methods, raw material is general food, without additional preparation, simply easily
?.
2, the present invention provides the raw material long-term consumption of carbon quantum dot, and securely and reliably, carbon quantum dot easily obtains, the reaction time
Short, carbon quantum dot fluorescence intensity is strong, good biocompatibility, can be widely applied to bio-carrier field.
3, the present invention is obtained on the basis of repeatedly testing repeatedly, using the side of THz wave assisted extraction degreasing
Method increases the recovery rate of carbon quantum dot in water-soluble macromolecule package, simultaneously because the demulsification of Terahertz, makes grease two
It mutually preferably separates, achievees the purpose that degreasing.The advantage operated in this way is, first is that increasing the recovery rate of carbon quantum dot；Two
It is first to remove grease, avoids the presence of a large amount of greases in extracting, be conducive to the extraction and purifying of carbon quantum dot；Three are that of avoiding
Later period removes grease using a large amount of organic solvents, saves organic solvent.
4, THz wave assisted extraction degreasing combination ultrasonic wave Assisted Ethanol extracts, and makes the carbon quantum dot in water phase and alcohol phase
To greatest extent extraction, this extracting method, than conventional method carbon quantum dot yield improve 15%, fluorescence intensity improve 20% with
On, organic solvent, green are not used, environmental protection is conducive to the application of carbon dots.
5, carbon quantum dot provided by the invention can indicate Maillard reaction degree, by fluorescence intensity, add to adjust
Work technique realizes the control to food processing process, reduces the generation of hazardous material, ensure food safety.
Specific embodiment
Below by specific implementation example, the present invention will be further described.
Fermented soya bean canned fish used in following embodiments is bought in Guangdong sweet bamboo jar head Co., Ltd: the purchase of chrysanthemum canned fish
Xiamen Gulong Food Co., Ltd.；Phoenix tail canned fish is bought in Shunde District, Foshan City Guangdong canned flower Food Co., Ltd；Broiled River Eel
Can is bought in Guangdong Hypon tinned food Co., Ltd.
Embodiment 1:
S1, raw material crush: the flesh of fish in 500g fermented soya bean canned fish is ground into 0.5cm × 0.5cm × 1cm fish block；
S2, THz wave assisted extraction degreasing:
It is primary to extract: pure water is added according to solid-liquid ratio 1:3g/ml in flesh of fish fritter obtained in step S1, it is primary to stir
30min is extracted, progress THz wave processing while primary stirring, the THz wave frequency 0.18THz, power 20KW,
Filtering, obtains the flesh of fish 1 and filtrate 1；
Second extraction: pure water is added according to solid-liquid ratio 1:1g/ml in the flesh of fish 1, after secondary agitation extracts 10min, secondary
THz wave processing, the THz wave frequency 0.18THz, power 20KW are carried out while stirring, filtering obtains the flesh of fish and filtrate
2, merge the filtrate 1 and filtrate 2；
S3, by the filtrate in step S2,4 DEG C, 8000r/min, be centrifuged 10min, remove grease, obtain aqueous extract；
S4, the extraction of ultrasonic wave Assisted Ethanol: by the gained flesh of fish in step S2 according to solid-liquid ratio 1:3g/ml, quality point is added
The ethyl alcohol that number is 100%, while utilizing Ultrasonic Wave-Assisted Extraction, ultrasonic frequency 80Hz, extraction time 0.5h；It filters,
Take filtrate；
S5, concentration: gained filtrate in the aqueous extract and step S4 in step S3 is merged, 40 DEG C, vacuum degree-
0.1MPa is concentrated into the 1/15 of original volume, obtains concentrate；
S6, alcohol precipitation removal of impurities: the second that the mass fraction of its 6 times of volumes is 95% is added in concentrate obtained in step S5
Alcohol at 4 DEG C, stands 10h；4 DEG C, 8000r/min are centrifuged 10min, take supernatant；
S7, evaporation and concentration: by supernatant obtained in step S6 carry out rotary evaporation, 50 DEG C, revolving speed 30r/min, very
Reciprocal of duty cycle -0.1MPa is concentrated into the 1/6 of original volume, obtains concentrate；
S8, dialysis purification: concentrate obtained in step S7 being placed in the bag filter of 1KDa molecular weight, uses 5 times of bodies
Long-pending deionized water dialysis, every 4h change a deionized water, change water 4 times, solution in bag taking；
S9, centrifugation: it by dialyzate obtained in step S8 under the revolving speed of 8000r/min, is centrifuged 10 minutes, takes supernatant
Liquid；
S10, freeze-drying: by gained supernatant in step S9, freeze-drying, -45 DEG C of shelf temperature, vacuum degree≤5Pa is dry
Time for 24 hours, obtains the carbon quantum dot with photoluminescent property.
The present embodiment obtains carbon quantum dot 4.95g, and fluorescence intensity is 2880 (1mg/ml carbon quantum dot aqueous solutions).
Embodiment 2:
S1, raw material crush: the flesh of fish in 500g chrysanthemum canned fish is ground into 1cm × 1cm × 1cm fish block；
S2, THz wave assisted extraction degreasing:
It is primary to extract: pure water is added according to solid-liquid ratio 1:1g/ml in flesh of fish fritter obtained in step S1, it is primary to stir
20min is extracted, carries out THz wave processing while the primary stirring, the THz wave frequency 0.3THz, power 40KW,
Filtering, obtains the flesh of fish 1 and filtrate 1；
Second extraction: pure water is added according to solid-liquid ratio 1:5g/ml in the flesh of fish 1, and secondary agitation extracts 30min, described secondary
THz wave processing, the THz wave frequency 0.3THz, power 40KW are carried out while stirring, filtering obtains the flesh of fish and filtrate
2, merge the filtrate 1 and filtrate 2；
S3, by the filtrate in step S2,4 DEG C, 8000r/min, be centrifuged 10min, remove grease, obtain aqueous extract；
S4, the extraction of ultrasonic wave Assisted Ethanol: by the gained flesh of fish in step S2 according to solid-liquid ratio 1:1g/ml, quality point is added
The ethanol water that number is 60%, while utilizing Ultrasonic Wave-Assisted Extraction, ultrasonic frequency 20Hz, extraction time 3h；It takes out
Filter, takes filtrate；
S5, concentration: gained filtrate in the aqueous extract and step S4 in step S3 is merged, 60 DEG C, vacuum degree-
0.08MPa is concentrated into the 1/25 of original volume, obtains concentrate；
S6, alcohol precipitation removal of impurities: the second that the mass fraction of its 6 times of volumes is 80% is added in concentrate obtained in step S5
Alcohol at 4 DEG C, stands 10h；4 DEG C, 8000r/min are centrifuged 10min, take supernatant；
S7, evaporation and concentration: by supernatant obtained in step S6 carry out rotary evaporation, 70 DEG C, revolving speed 60r/min, very
Reciprocal of duty cycle -0.08MPa is concentrated into the 1/10 of original volume, obtains concentrate；
S8, dialysis purification: concentrate obtained in step S7 being placed in the bag filter of 1KDa molecular weight, uses 15 times of bodies
Long-pending deionized water dialysis, every 4h change a deionized water, change water 3 times, solution in bag taking；
S9, centrifugation: it by dialyzate obtained in step S8 under the revolving speed of 8000r/min, is centrifuged 10 minutes, takes supernatant
Liquid；
S10, freeze-drying: by gained supernatant in step S9,60 DEG C of shelf temperature, vacuum degree≤5Pa, drying time 12h is obtained
To the carbon quantum dot with photoluminescent property.
The present embodiment obtains carbon quantum dot and obtains carbon quantum dot 2.89g, and fluorescence intensity is 940 (1mg/ml carbon quantum dot water
Solution)
Embodiment 3:
S1, raw material crush: the flesh of fish in 500g phoenix tail canned fish is ground into 2cm × 2cm × 2cm fish block；
S2, THz wave assisted extraction degreasing: flesh of fish fritter obtained in step S1 is added according to solid-liquid ratio 1:2g/ml
10min is extracted in pure water, primary stirring, and primary stirring while carries out THz wave processing, the THz wave frequency
0.25THz, power 30KW, filtering, obtain the flesh of fish and filtrate 1；Pure water, secondary agitation is added according to solid-liquid ratio 1:3g/ml in the flesh of fish
20min is extracted, THz wave processing, the THz wave frequency 0.25THz, power are carried out while the secondary agitation
30KW, filtering, obtains the flesh of fish and filtrate 2, merges the filtrate 1 and filtrate 2；
S3, by the filtrate in step S2,4 DEG C, 8000r/min, be centrifuged 10min, remove grease, obtain aqueous extract；
S4, the extraction of ultrasonic wave Assisted Ethanol: by the gained flesh of fish in step S2 according to solid-liquid ratio 1:2g/ml, quality point is added
The ethanol water that number is 80%, while utilizing Ultrasonic Wave-Assisted Extraction, ultrasonic frequency 20Hz, extraction time 2h；It takes out
Filter, takes filtrate；
S5, concentration: gained filtrate in the aqueous extract and step S4 in step S3 is merged, 50 DEG C, vacuum degree-
0.09MPa is concentrated into the 1/20 of original volume, obtains concentrate；
S6, alcohol precipitation removal of impurities: the second that the mass fraction of its 5 times of volumes is 90% is added in concentrate obtained in step S5
Alcohol at 8 DEG C, stands 18h；4 DEG C, 8000r/min are centrifuged 10min, take supernatant；
S7, evaporation and concentration: by supernatant obtained in step S6,60 DEG C, revolving speed 40r/min, vacuum degree -0.09MPa,
It is concentrated into the 1/8 of original volume, obtains concentrate；
S8, dialysis purification: concentrate obtained in step S7 being placed in the bag filter of 1KDa molecular weight, uses 10 times of bodies
Long-pending deionized water dialysis, every 4h change a deionized water, change water 3 times, solution in bag taking；
S9, centrifugation: it by dialyzate obtained in step S8 under the revolving speed of 8000r/min, is centrifuged 10 minutes, takes supernatant
Liquid；
S10, freeze-drying: by gained supernatant in step S9,10 DEG C of shelf temperature, vacuum degree≤5Pa, drying time 18h is obtained
To the carbon quantum dot with photoluminescent property.
The present embodiment obtains carbon quantum dot 3.2g, and fluorescence intensity is 860 (1mg/ml carbon quantum dot aqueous solutions).
Embodiment 4:
S1, raw material crush: the flesh of fish in 500g roast eel canned fish is ground into 0.5cm × 0.5cm × 0.5cm fish
Block；
S2, THz wave assisted extraction degreasing:
It is primary to extract: pure water is added according to solid-liquid ratio 1:5g/ml in flesh of fish fritter obtained in step S1, it is primary to stir
20min is extracted, carries out THz wave processing while the primary stirring, the THz wave frequency 0.2THz, power 20KW,
Filtering, obtains the flesh of fish 1 and filtrate 1；
Pure water is added according to solid-liquid ratio 1:2g/ml in the flesh of fish 1, and secondary agitation extracts 20min, while the secondary agitation
THz wave processing, the THz wave frequency 0.25THz, power 30KW are carried out, filtering obtains the flesh of fish and filtrate 2, described in merging
Filtrate 1 and filtrate 2；
S3, by the filtrate in step S2,4 DEG C, 8000r/min, be centrifuged 10min, remove grease, obtain aqueous extract；
S4, the extraction of ultrasonic wave Assisted Ethanol: by the gained flesh of fish in step S2 according to solid-liquid ratio 1:3g/ml, quality point is added
The ethanol water that number is 90%, while utilizing Ultrasonic Wave-Assisted Extraction, ultrasonic frequency 60Hz, extraction time 1.5h；
It filters, takes filtrate；
S5, concentration: gained filtrate in the aqueous extract and step S4 in step S3 is merged, 45 DEG C, vacuum degree-
0.09MPa is concentrated into the 1/18 of original volume, obtains concentrate；
S6, alcohol precipitation removal of impurities: the second that the mass fraction of its 5 times of volumes is 90% is added in concentrate obtained in step S5
Alcohol at 15 DEG C, is stood for 24 hours；4 DEG C, 8000r/min are centrifuged 10min, take supernatant；
S7, evaporation and concentration: by supernatant obtained in step S6,50 DEG C, revolving speed 40r/min, vacuum degree -0.09MPa,
It is concentrated into the 1/9 of original volume, obtains concentrate；
S8, dialysis purification: concentrate obtained in step S7 being placed in the bag filter of 1KDa molecular weight, uses 6 times of bodies
Long-pending deionized water dialysis, every 4h change a deionized water, change water 3 times, solution in bag taking；
S9, centrifugation: it by dialyzate obtained in step S8 under the revolving speed of 8000r/min, is centrifuged 10 minutes, takes supernatant
Liquid；
S10, freeze-drying: by gained supernatant in step S9,30 DEG C of shelf temperature, vacuum degree≤5Pa, drying time 12h is obtained
To the carbon quantum dot with photoluminescent property.
The present embodiment obtains carbon quantum dot 4.2g, and fluorescence intensity is 1300 (1mg/ml carbon quantum dot aqueous solutions).
Comparative example 1:
S1, raw material crush: the flesh of fish in 500g fermented soya bean canned fish is ground into 0.5cm × 0.5cm × 1cm fish block；
S2, the extraction of ultrasonic wave Assisted Ethanol:
It is primary to extract: by the gained flesh of fish in step S1 according to solid-liquid ratio 1:3g/ml, the second that mass fraction is 100% is added
Alcohol solution, while utilizing Ultrasonic Wave-Assisted Extraction, ultrasonic frequency 40Hz, time 3h；It filters, obtains the flesh of fish 1 and filtrate
1；
The ethanol water that mass fraction is 80% is added by the flesh of fish 1 according to solid-liquid ratio 1:3g/ml in second extraction, ultrasound
Wave frequency rate is 80Hz, extraction time 2h；It filters, takes filtrate 2；Merge the filtrate 1 and filtrate 2；
S3, concentration: by gained filtrate in step S2, at 40 DEG C, vacuum degree -0.1MPa is concentrated into the 1/8 of original volume,
Obtain concentrate；
S4, organic solvent degreasing: by concentrate obtained in step S3: the ethyl acetate of its 3 times of volumes is added, acutely shakes
Dynamic 10min, stands 20min, goes ethyl acetate phase, stay water phase.It extracts 6 times repeatedly, obtains the water containing carbon dots of removal grease
Phase solution；This comparative example uses ethyl acetate 3375g altogether；
S5, alcohol precipitation removal of impurities: the second that the mass fraction of its 3 times of volumes is 95% is added in aqueous phase solution obtained in step S4
Alcohol at 4 DEG C, stands 12h；At 4 DEG C, 8000r/min, centrifugation 10min takes supernatant；
S6, evaporation and concentration: supernatant obtained in step S5 is concentrated into the 1/4 of original volume, obtained by rotary evaporation
Concentrate；Wherein, the temperature of the rotary evaporation is 50 DEG C, revolving speed 60r/min；
S7, dialysis purification: concentrate obtained in step S6 being placed in the bag filter of 1KDa molecular weight, uses 5 times of bodies
Long-pending deionized water dialysis, every 4h change a deionized water, change water 3 times, solution in bag taking；
S8 centrifugation: it by dialyzate obtained in step S7 under the revolving speed of 8000r/min, is centrifuged 10 minutes, takes supernatant；
S9, freeze-drying: by gained supernatant in step S8, freeze-drying, -45 DEG C of shelf temperature, vacuum degree≤5Pa is dry
Time for 24 hours, obtains the carbon quantum dot with photoluminescent property.
Carbon quantum dot 3.98g is obtained in this comparative example, fluorescence intensity is 2200 (1mg/ml carbon quantum dot aqueous solutions).
In conclusion the fat content of canned fish is higher, using the method for first degreasing, be conducive to keep subsequent carbon quantum dot
Extraction and purifying, carbon quantum dot yield improve 15%, fluorescence intensity improve 20% or more, be conducive to the application of carbon dots.
The foregoing is only a preferred embodiment of the present invention, but scope of protection of the present invention is not limited thereto,
Anyone skilled in the art within the technical scope of the present disclosure, according to the technique and scheme of the present invention and its
Inventive concept is subject to equivalent substitution or change, should be covered by the protection scope of the present invention.
Claims (10)
1. a kind of method for extracting fluorescent carbon quantum dot from canned fish, which is characterized in that comprising steps of
S1, raw material crush: the flesh of fish in canned fish is ground into fritter；
S2, THz wave assisted extraction degreasing:
It is primary to extract: by flesh of fish fritter obtained in step S1 according to solid-liquid ratio 1:(1~5) g/ml addition pure water, is once stirred
Mix 10~30min, primary stirring while carries out THz wave processing, and filtering obtains the flesh of fish 1 and filtrate 1；
Second extraction: the flesh of fish 1 is according to solid-liquid ratio 1:(1~5) g/ml addition pure water, secondary agitation extracts 10~30min, described
THz wave processing is carried out while secondary agitation, filtering obtains the flesh of fish and filtrate 2；Merge the filtrate 1 and filtrate 2, must filter
Liquid；
S3, filtrate obtained by step S2 is centrifuged, removes grease, obtains aqueous extract；
S4, the extraction of ultrasonic wave Assisted Ethanol: by the flesh of fish obtained by step S2 according to solid-liquid ratio 1:(1~3) g/ml, mass fraction is added
For 60%~100% ethyl alcohol, ultrasonication, the ultrasonic frequency is 20~80Hz, and the time is 0.5~3h；It filters, takes
Filtrate；
S5, concentration: filtrate obtained by aqueous extract obtained by step S3 and step S4 is merged, the 1/15~1/ of original volume is concentrated into
25, obtain concentrate；
S6, alcohol precipitation removal of impurities: the second that the mass fraction of its 3~6 times of volumes is 80%~95% is added in concentrate obtained by step S5
Alcohol, at 4~15 DEG C, stand 10~for 24 hours；Centrifuging and taking supernatant；
S7, evaporation and concentration: supernatant obtained by step S6 is concentrated into the 1/6~1/10 of original volume, obtains concentrate through pervaporation；
S8, dialysis purification: dialysing to the resulting concentrate of step S7 using deionized water, the solution after taking dialysis；
S9, centrifugation: by the solution centrifuging and taking supernatant after dialysis obtained by step S8；
S10, freeze-drying: by supernatant obtained by step S9, freeze-drying obtains the carbon quantum dot with photoluminescent property.
2. the method for fluorescent carbon quantum dot is extracted from canned fish according to claim 1, which is characterized in that described in step S1
Fritter specifically: 0.5cm × 0.5cm × 0.5cm~2cm × 2cm × 2cm.
3. the method for fluorescent carbon quantum dot is extracted from canned fish according to claim 1, which is characterized in that described in step S1
Canned fish is one of chrysanthemum canned fish, dace with black bean can, roast eel canned fish, phoenix tail canned fish.
4. the method for fluorescent carbon quantum dot is extracted from canned fish according to claim 1, which is characterized in that described in step S2
The frequency of THz wave is 0.18~0.3THz, and power is 20~40KW.
5. the method for fluorescent carbon quantum dot is extracted from canned fish according to claim 1, which is characterized in that described in step S3
Centrifugation are as follows: 4 DEG C, 8000r/min are centrifuged 10min.
6. the method for fluorescent carbon quantum dot is extracted from canned fish according to claim 1, which is characterized in that described in step S5
Concentration is vacuum concentration, design parameter are as follows: 40~60 DEG C, vacuum degree -0.08~-0.1MPa.
7. the method for fluorescent carbon quantum dot is extracted from canned fish according to claim 1, which is characterized in that described in step S6
Centrifugation are as follows: 4 DEG C, 8000r/min are centrifuged 10min.
8. the method for fluorescent carbon quantum dot is extracted from canned fish according to claim 1, which is characterized in that described in step S7
It is evaporated to rotary evaporation, design parameter are as follows: 50~70 DEG C of rotating evaporation temperature, revolving speed is 30~60r/min, vacuum degree -0.08
~-0.1MPa.
9. the method for fluorescent carbon quantum dot is extracted from canned fish according to claim 1, which is characterized in that step S8 is specific
Are as follows: concentrate obtained by step S7 is placed in the bag filter with 1KDa molecular weight, using the deionized water of 5~15 times of volumes to it
It dialyses, every 4h changes a deionized water, changes water 3~5 times.
10. the method for fluorescent carbon quantum dot is extracted from canned fish according to claim 1, which is characterized in that step S10 institute
State freeze-drying specifically: shelf temperature -45~60 DEG C, vacuum degree≤5Pa, drying time 12~for 24 hours.
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| CN113462192A (en) * | 2021-07-01 | 2021-10-01 | 上海禧蓝纺织品有限公司 | Extraction and dyeing method of plant dye and plant mordant |
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