CN108195830A - A kind of visible detection method for trace copper ion - Google Patents
A kind of visible detection method for trace copper ion Download PDFInfo
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- CN108195830A CN108195830A CN201711375757.9A CN201711375757A CN108195830A CN 108195830 A CN108195830 A CN 108195830A CN 201711375757 A CN201711375757 A CN 201711375757A CN 108195830 A CN108195830 A CN 108195830A
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Abstract
The invention discloses a kind of visible detection methods for trace copper ion.The main points of this method are the cellulose base sensor Adsorption of Cu to have both schiff base structure and amino-functional group2+, by amino to Cu2+Chelation and schiff bases isomerization colour developing, realize the Visual retrieval to trace copper ion.Copper ion detection method of the present invention has the characteristics that the cellulose base sensor of easy to operate, high sensitivity, visualization, low cost, and gained can be prepared into liquid condition, pulverulence and Test paper state on demand, is used directly for trace Cu2+Visual retrieval in aqueous solution and biological fluid.
Description
Technical field
The present invention relates to one kind to be used for trace Cu2+The method of Visual retrieval, belongs to analytical chemistry field.
Background technology
Copper plays a crucial role in human life activity, is the indispensable metallic element of human body.However, people
The content of copper also has a stringent standard in body, and the normal content of copper ion of urine is 20-40mg/ days in human body, serum copper normal value
14.7~20.5mmol/L.Its excessive concentration too low can all have an adverse effect to human body.As copper ion lacks meeting in human body
Influence the activity (such as superoxide dismutase, dopamine β-hydroxylase, tyrosinase) of many enzymes and the metabolism of cell；
Copper ion can excessively lead to functional disturbances of gastrointestinal tract, liver and renal function metabolism disorder, hemolytic anemia and nervus retrogression disease
The generation of disease, such as Wilson's syndrome and alzheimer's disease.Copper can excessively cause air, water body and soil dirty in environment
Dye, serious harm is constituted to ecological environment and food security, enters human body eventually by food chain and then human body is generated
Harm.Environmental Protection Agency USA provides the content of copper in drinking water ion no more than 1.3ppm, and China environmental protection office is similary
Provide the content of copper in drinking water ion no more than 2ppm.Therefore quick, easy copper ion detection method is established, in human body
Health, environment measuring etc. have a very important significance.
Currently used copper detection method has graphite furnace atomic absorption spectrometry, ultraviolet spectrophotometry, inductive coupling etc.
Gas ions mass spectrography and fluorescent spectrometry etc..These methods can meet the detection of above-mentioned standard because of relatively good sensitivity；So
And these methods are almost required for expensive instrument and quite professional operation, are only suitable for completing detection in laboratory.It compares
In conventional method, colorimetric method with it is quick, portable, at low cost, intuitive, can the advantages such as field assay cause that numerous researchers' is emerging
Interest.Such as patent CN 104897664A, copper ion is adsorbed by ligand of porous polyaspartic acid hydrogels, under alkaline condition,
With copper ion complexing biuret reaction colour developing occurs for porous polyaspartic acid hydrogels.But it is needed in detection process
The effect really detected in real time is not achieved in alkaline environment.The designs such as Fu Fengfu have been synthesized to be derived with rhodamine B spirocyclic lactams
Object is Cu2+Probe is identified, with reference to Fe3O4Magnetic nano-particle is realized to Cu2+Visual retrieval, but the method synthesis step
Cumbersome, detection time is relatively long, is not suitable for the detection of scene copper ion.More than research background and real current situation are based on, is needed
Develop the material that a kind of raw material is cheap, environmentally protective, particularly a kind of material can be used for efficiently quick Visual retrieval water-soluble
The sensor of trace copper ion in liquid and biological fluid.
Invention content
For the disadvantages described above or Improvement requirement of the prior art, the purpose of the present invention is realize to the visual of trace copper ion
Change detection, which has the characteristics that quick, simple, high sensitivity, high specific, low cost, can
For the Visual retrieval of copper ion in aqueous solution and biological fluid.
To achieve the above object, technical solution of the invention is：
First, it is a kind of to be used for trace Cu2+The cellulose base sensor of Visual retrieval：
Cellulose base sensor has both schiff base structure and amino-functional group, form be liquid or powder either
Based on the Test paper made by liquid cellulose based sensor.
The present invention is using the cellulose base sensor to Cu2+It is adsorbed, by amino (N-H) to Cu2+Chelating make
It is developed the color with the isomerization with schiff base structure (C=N), realizes the Visual retrieval to copper ion.
The cellulose base sensor is formed including polyethyleneimine, ethylenediamine or lysine and its derivative
Modified cellulose.
The derivative of the lysine specifically includes polylysine and l-Lysine hydrochloride.
2nd, it is a kind of to be used for trace Cu2+The preparation method of the cellulose base sensor of Visual retrieval, it is characterised in that method
Step is：
Cellulose and sodium metaperiodate are dissolved into the aqueous solution of 7wt%NaOH and 12wt% urea, adjust mixed solution
PH after heating water bath, adding amino compound, the reaction was continued, the centrifugation of obtained reaction product, isolated supernatant liquor
And lower sediment thing, using supernatant liquor as the liquid form of cellulose base sensor, using lower sediment thing as cellulose base
The powder morphology of sensor prepares Test paper using infusion process as maceration extract using supernatant liquor and is sensed as cellulose base
The Test paper form of device, so as to obtain the three of cellulose base sensor kinds of states.
The amino compound relies ammonia for polyethyleneimine, ethylenediamine, lysine, poly-D-lysine or L- hydrochloric acid
Acid.
The method is specifically：The 7wt%NaOH and 12wt% that 2g celluloses and 2g sodium metaperiodates are dissolved into 60mL urinate
In the aqueous solution of element, adjustment mixed solution pH is 4, and mixed solution then is added in 2g aminos in 60 DEG C of heating water baths 4 hours
The reaction was continued 3 hours for compound, and obtained reaction product centrifuges 10min, isolated supernatant liquor under the conditions of 8000rpm
And lower sediment thing.
The reaction product is cellulose graft polyethyleneimine-modified cellulose, cellulose graft ethylenediamine is modified fibre
Tie up element, the lysine modified cellulose of cellulose graft, cellulose graft poly-D-lysine modified cellulose, cellulose graft L- salt
The lysine modified cellulose of acid.
3rd, the first is used for trace Cu2+The method of Visual retrieval, method and step are：
First, by any liquid of claim 1-2 or pulverulence cellulose base sensor or claim 3
The liquid or pulverulence cellulose base sensor that the method is prepared are added to containing the molten of known various concentration copper ion
In liquid, 5min colour developings are stood, various concentration copper ion solution corresponds to different color changes, and color change is from colourless to dark green
Color, colourless to represent a concentration of zero, bottle green represents concentration highest, establishes the corresponding various criterion color of various concentration copper ion；
Then, the cellulose base sensor of liquid condition and pulverulence is added in the solution to be measured of copper ions,
It stands 5min solution to develop the color, be compared with the color and reference colour of display, the corresponding concentration for obtaining copper ion.
4th, it is used for trace Cu second2+The method of Visual retrieval, method and step are：
First, the solution containing known various concentration copper ion is added dropwise respectively in any detections of claim 1-2
The Test paper that test paper or claim 3 the method are prepared stands 5min colour developings, various concentration copper ion solution pair
The color change of different test strips is answered, color change is faint yellow to represent concentration zero, bottle green from faint yellow to bottle green
Concentration highest is represented, establishes the corresponding various criterion color of various concentration copper ion；
Then, the solution to be measured of copper ions is added drop-wise on Test paper, stands 5min Test papers and develop the color, with aobvious
The color and reference colour shown are compared, the corresponding concentration for obtaining copper ion.
Trace copper ion detection of the cellulose base sensor suitable for water, artificial urine and blood plasma.The present invention's
Cellulose base sensor is suitable for complex biological body fluid, be especially adapted for use in artificial urine and blood plasma containing the molten of complex material
Liquid carries out trace copper ion detection, and copper ion relevant disease (hepatolenticular degeneration, Menkes disease etc.) tentatively can be examined with this
It is disconnected.
The present invention does not need to fluorescein, does not need to complicated detection process, the method for the present invention letter compared to traditional detection method
It is single effective.
The present invention is using amino (N-H) to Cu2+Chelation and schiff bases (C=N) isomerization colour developing it is (colourless
To bottle green) the characteristics of, realize the Visual retrieval to trace copper ion.The copper ion visible detection method have it is quick,
Simply, the features such as high sensitivity, high specific, low cost, the visualization inspection available for copper ion in aqueous solution and biological fluid
It surveys.
In general, the above technical scheme conceived by the present invention compared with prior art, can obtain following
Advantageous effect：
1. detection method response of the present invention is fast, one-time detection only needs the 5min times.
2. detection method of the present invention has high sensitivity, the copper ion concentration down to 1ppm is can detect, can be met
The testing requirements of relevant criterion, available for Cu in water environment, drinking water and biological fluid2+Field quick detection.
3. detection method of the present invention has good specificity, the cellulose base sensor is only to Cu2+There is colour developing
Reaction, has investigated 10 kinds of common ion (Zn2+、Mn2+、Fe3+、Ca2+、Mg2+、Pb2+、 Na+、Ag+、Cd2+、Al3+), do not cause
Interference.
4. cellulose base sensor can be prepared into liquid, powder by detection method of the present invention according to different demands
End and Test paper have wider application range.
5. detection method of the present invention is simple, it can determine whether copper ion concentration range with bore hole, do not need to by big
Type detecting instrument is suitble to the field quick detection of copper ion.
6. detection method of the present invention can add in prepare liquid according to liquid or pulverulence cellulose base sensor
The color or the color shown on Test paper is added dropwise come to copper ion in testing liquid according to testing liquid that body is shown
Concentration carry out sxemiquantitative.
7. detection method of the present invention uses one kettle way that cellulose base sensor is prepared with cellulose and poly- second
Alkene imines is raw material, does not have harmful substance generation in preparation process, will not generate secondary pollution to environment.
Description of the drawings
Fig. 1 be by containing 0,2,5,8, the copper ion blood plasma of 10ppm the cellulose base sensor that is prepared in the present invention is added dropwise
Test paper on mock standard color made by the different colours that show colorimetric card schematic diagram.
Specific embodiment
The technological means and advantage taken further to illustrate the present invention, below in conjunction with the implementation of the present invention
Example and its attached drawing are specifically described.
The embodiment of the present invention is as follows：
Embodiment 1：
(1) 2g celluloses and 2g sodium metaperiodates are dissolved into the aqueous solution of 7wt%NaOH and 12wt% urea of 60mL,
It is 4 to adjust mixed solution pH, then by mixed solution in 60 DEG C of heating water baths 4 hours, adds in 2g polyethyleneimines the reaction was continued 3
Hour, obtained reaction product centrifuges 10min, isolated supernatant liquor and lower sediment thing under the conditions of 8000rpm.With
Liquid form of the supernatant liquor as cellulose base sensor, using lower sediment thing as the powder shape of cellulose base sensor
State prepares Test paper as the Test paper shape of cellulose base sensor using supernatant liquor as maceration extract using infusion process
State, so as to obtain the three of cellulose base sensor kinds of states.
(2) 2ml is taken to be added to 20ml containing known various concentration the liquid condition cellulose base sensor described in step (1)
In the solution of copper ion (0ppm, 2ppm, 4ppm, 6ppm, 8ppm, 10ppm), stand 5min solution and develop the color, various concentration copper
Solion corresponds to different color changes, and color change is from colourless to bottle green, and colourless to represent a concentration of zero, bottle green represents
Concentration highest, establishes the corresponding various criterion color of various concentration copper ion, i.e. 0ppm correspond to it is colourless, 2ppm correspond to it is faint yellow,
4ppm corresponds to light green, and 6ppm corresponds to yellow green, and 8ppm corresponds to green, and 10ppm corresponds to bottle green；
(3) water sample to be measured that 20ml is taken to contain trace copper ion adds in the liquid condition cellulose base described in step (1) and passes
Sensor 2ml, stand 5min solution be shown as light green, according to the reference colour obtained by step (2) Copper in Water Samples to be measured from
A concentration of 4ppm of son.
The present embodiment is simultaneously detected water sample to be measured using AA-110 models flame atomic absorption spectrophotometer, and gained is treated
The copper ion concentration for surveying water sample is 4.1721ppm, is 4.3% with errors of the present invention, illustrates that the method for the present invention simply has
Effect measures accurate.The setting of AA-110 model Atomic Absorption Spectrometers basic parameter is as follows：Wavelength is 324.75nm, and slit width is
0.7nm, time constant 0.1s, electric current 10mA, lighting mode go background for non-deuterium lamp, and gas flow 2.0L/min is helped
Gas flow is 15.0L/min, flame pattern Air-C2H2。
Embodiment 2：
(1) 2g celluloses and 2g sodium metaperiodates are dissolved into the aqueous solution of 7wt%NaOH and 12wt% urea of 60mL,
It is 4 to adjust mixed solution pH, and then by mixed solution in 60 DEG C of heating water baths 4 hours, it is small to add in 2g ethylenediamines the reaction was continued 3
When, obtained reaction product centrifuges 10min, isolated supernatant liquor and lower sediment thing under the conditions of 8000rpm.With upper strata
Liquid form of the clear liquid as cellulose base sensor, using lower sediment thing as the powder morphology of cellulose base sensor, with
Supernatant liquor prepares Test paper form of the Test paper as cellulose base sensor for maceration extract using infusion process, from
And obtain three kinds of states of cellulose base sensor.
(2) 20mg is taken to be added to containing known various concentration the pulverulence cellulose base sensor described in step (1) one
In the artificial urine of copper ion (0ppm, 2ppm, 4ppm, 6ppm, 8ppm, 10ppm), stand 5min solution and develop the color, it is different dense
Degree copper ion solution corresponds to different color changes, and color change is from colourless to bottle green, colourless to represent a concentration of zero, bottle green
Concentration highest is represented, establishes the corresponding various criterion color of various concentration copper ion, is i.e. 0ppm corresponds to colourless, and 2ppm corresponds to yellowish
Color, 4ppm correspond to light green, and 6ppm corresponds to yellow green, and 8ppm corresponds to green, and 10ppm corresponds to bottle green；
(3) urine sample to be measured that 20ml is taken to contain trace copper ion adds in the pulverulence cellulose base described in step (1) and passes
Sensor 20mg stands 5min solution and is shown as faint yellow, according to the reference colour obtained by step (2) in the urine sample to be measured copper from
A concentration of 2ppm of son.
The present embodiment is simultaneously detected urine sample to be measured using AA-110 models flame atomic absorption spectrophotometer, and gained is treated
The copper ion concentration for surveying urine sample is 2.0971ppm, is 4.9% with errors of the present invention, illustrates that the method for the present invention simply has
Effect measures accurate.The setting of AA-110 model Atomic Absorption Spectrometers basic parameter is as follows：Wavelength is 324.75nm, and slit width is
0.7nm, time constant 0.1s, electric current 10mA, lighting mode go background for non-deuterium lamp, and gas flow 2.0L/min is helped
Gas flow is 15.0L/min, flame pattern Air-C2H2。
Embodiment 3：
(1) 2g celluloses and 2g sodium metaperiodates are dissolved into the aqueous solution of 7wt%NaOH and 12wt% urea of 60mL,
It is 4 to adjust mixed solution pH, and then by mixed solution in 60 DEG C of heating water baths 4 hours, it is small to add in 2g ethylenediamines the reaction was continued 3
When, obtained reaction product centrifuges 10min, isolated supernatant liquor and lower sediment thing under the conditions of 8000rpm.With upper strata
Liquid form of the clear liquid as cellulose base sensor, using lower sediment thing as the powder morphology of cellulose base sensor, with
Supernatant liquor prepares Test paper form of the Test paper as cellulose base sensor for maceration extract using infusion process, from
And obtain three kinds of states of cellulose base sensor.
(2) by blood plasma (0ppm, 2ppm, 5ppm, 8ppm, 10ppm) of the 0.5ml containing known various concentration copper ion respectively
It is added dropwise in the Test paper described in step (1), stands 5min colour developings, various concentration copper ion solution corresponds to different Test papers
The color change of item, color change is from faint yellow to bottle green, and faint yellow to represent concentration zero, bottle green represents concentration highest, builds
The corresponding various criterion color of vertical various concentration copper ion, i.e. 0ppm correspond to faint yellow, and 2ppm corresponds to buff, and 5ppm corresponds to pale green
Color, 8ppm correspond to green, and 10ppm corresponds to bottle green (as shown in Figure 1).
(3) the test plasma sample that 0.5ml contains trace copper ion is taken, is added dropwise in the test strip described in step (1),
Stand 5min test strips and be shown as yellow green, according to the reference colour obtained by step (2) in the test plasma sample copper from
A concentration of 2ppm of son.
The present embodiment is simultaneously detected urine sample to be measured using AA-110 models flame atomic absorption spectrophotometer, and gained is treated
The copper ion concentration for surveying blood plasma sample is 2.1127ppm, is 5.6% with errors of the present invention, illustrates that the method for the present invention is simple
It is accurate effectively to measure.The setting of AA-110 model Atomic Absorption Spectrometers basic parameter is as follows：Wavelength is 324.75nm, slit width
For 0.7nm, time constant 0.1s, electric current 10mA, lighting mode goes background for non-deuterium lamp, gas flow 2.0L/min,
Combustion air current amount is 15.0L/min, flame pattern Air-C2H2。
As seen from the above-described embodiment, copper ion detection method of the present invention has easy to operate, high sensitivity, visualization, low
The features such as cost, and the cellulose base sensor of gained can be prepared into liquid condition, pulverulence and Test paper on demand
State is used directly for trace Cu2+Visual retrieval in aqueous solution and biological fluid.
Listed above is only specific embodiments of the present invention.It is clear that the invention is not restricted to above embodiment, may be used also
With there are many deformations.All changes that those of ordinary skill in the art directly can export or associate from present disclosure
Shape is considered as protection scope of the present invention.
Claims (8)
1. one kind is used for trace Cu2+The cellulose base sensor of Visual retrieval, it is characterised in that：Cellulose base sensor has both
Schiff base structure and amino-functional group, form are that liquid or powder are either made based on liquid cellulose based sensor
Into Test paper.
It is 2. according to claim 1 a kind of for trace Cu2+The cellulose base sensor of Visual retrieval, feature exist
In：The cellulose base sensor includes the modification that polyethyleneimine, ethylenediamine or lysine and its derivative are formed
Cellulose.
3. trace Cu to be used for described in a kind of claim 12+The preparation method of the cellulose base sensor of Visual retrieval, feature
Being method and step is：Cellulose and sodium metaperiodate are dissolved into the aqueous solution of NaOH and urea, adjust the pH of mixed solution
Heating water bath afterwards, adding amino compound, the reaction was continued, and obtained reaction product centrifugation, isolated supernatant liquor is under
Layer sediment using supernatant liquor as the liquid form of cellulose base sensor, is sensed using lower sediment thing as cellulose base
The powder morphology of device prepares Test paper as cellulose base sensor using supernatant liquor as maceration extract using infusion process
Test paper form.
It is 4. according to claim 3 a kind of for trace Cu2+The preparation method of the cellulose base sensor of Visual retrieval,
It is characterized in that：The amino compound is polyethyleneimine, ethylenediamine, lysine, poly-D-lysine or L- hydrochloric acid
Lysine.
It is 5. according to claim 3 a kind of for trace Cu2+The preparation method of the cellulose base sensor of Visual retrieval,
It is characterized in that：The method is specifically：2g celluloses and 2g sodium metaperiodates are dissolved into the 7wt%NaOH and 12wt% of 60mL
In the aqueous solution of urea, adjustment mixed solution pH is 4, and mixed solution then is added in 2g amino in 60 DEG C of heating water baths 4 hours
The reaction was continued 3 hours for class compound, and obtained reaction product centrifuges 10min, isolated supernatant liquor under the conditions of 8000rpm
And lower sediment thing.
6. one kind is used for trace Cu2+The method of Visual retrieval, it is characterised in that method and step is：
It first, will be described in any liquid of claim 1-2 or pulverulence cellulose base sensor or claim 3
The liquid or pulverulence cellulose base sensor that method is prepared are added in the solution containing known various concentration copper ion,
5min colour developings are stood, various concentration copper ion solution corresponds to different color changes, and color change is colourless from colourless to bottle green
A concentration of zero is represented, bottle green represents concentration highest, establishes the corresponding various criterion color of various concentration copper ion；
Then, the cellulose base sensor of liquid condition and pulverulence is added in the solution to be measured of copper ions, stood
5min solution develops the color, and is compared with the color and reference colour of display, the corresponding concentration for obtaining copper ion.
7. one kind is used for trace Cu2+The method of Visual retrieval, it is characterised in that method and step is：
First, the solution containing known various concentration copper ion is added dropwise respectively in any Test papers of claim 1-2
Or the Test paper that claim 3 the method is prepared, 5min colour developings are stood, various concentration copper ion solution corresponds to not
The color change of same test strip, color change is from faint yellow to bottle green, and faint yellow to represent concentration zero, bottle green represents
Concentration highest establishes the corresponding various criterion color of various concentration copper ion；
Then, the solution to be measured of copper ions is added drop-wise on Test paper, stands 5min Test papers and develop the color, with display
Color and reference colour are compared, the corresponding concentration for obtaining copper ion.
8. fiber is prepared in any cellulose base sensors of claim 1-2 or claim 3 the method
The application of plain based sensor, it is characterised in that：Trace of the cellulose base sensor suitable for water, artificial urine and blood plasma
Copper ion detects.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201711375757.9A CN108195830B (en) | 2017-12-19 | 2017-12-19 | Visual detection method for trace copper ions |
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| CN201711375757.9A CN108195830B (en) | 2017-12-19 | 2017-12-19 | Visual detection method for trace copper ions |
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| CN110204734A (en) * | 2019-06-14 | 2019-09-06 | 陕西科技大学 | A kind of polyethyleneimine/salicylide modified cellulosic materials and its preparation method and application |
| CN110565440A (en) * | 2019-09-06 | 2019-12-13 | 陕西科技大学 | salicylaldehyde Schiff base/graphene oxide modified paper-based material and preparation method and application thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110204734A (en) * | 2019-06-14 | 2019-09-06 | 陕西科技大学 | A kind of polyethyleneimine/salicylide modified cellulosic materials and its preparation method and application |
| CN110204734B (en) * | 2019-06-14 | 2021-10-01 | 陕西科技大学 | Polyethyleneimine/salicylaldehyde modified cellulose material and preparation method and application thereof |
| CN110565440A (en) * | 2019-09-06 | 2019-12-13 | 陕西科技大学 | salicylaldehyde Schiff base/graphene oxide modified paper-based material and preparation method and application thereof |
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| Publication number | Publication date |
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| CN108195830B (en) | 2020-10-23 |
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