CN109444234A - A kind of production method of graphene brilliant cresyl blue urinary albumin test electrode - Google Patents
A kind of production method of graphene brilliant cresyl blue urinary albumin test electrode Download PDFInfo
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- CN109444234A CN109444234A CN201811233624.2A CN201811233624A CN109444234A CN 109444234 A CN109444234 A CN 109444234A CN 201811233624 A CN201811233624 A CN 201811233624A CN 109444234 A CN109444234 A CN 109444234A
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Abstract
The invention discloses a kind of production methods of graphene brilliant cresyl blue urinary albumin test electrode, comprising the following steps: the preparation of pet substrate；Graphene working electrode, reference electrode, the production to electrode；It uses print process that polymer insulation paint is printed in except insertion end and reaction zone are with the pet substrate of exterior domain, forms insulating layer；By crosslinking agent and urinary albumin selective reaction object solution, graphene working electrode, silver/silver chlorate are spread evenly across as reference electrode, carbon as the sample reaction zone to electrode in the method for spin coating, it is dried in 36-38 DEG C, then one layer of PVC insulating film is covered in reaction zone and form injection port, obtain graphene brilliant cresyl blue urinary albumin test electrode.Graphene brilliant cresyl blue urinary albumin of the invention has the advantages of time-consuming short, work efficiency is high when testing electrode detection；In addition, can accomplish the content for detecting urinary albumin in due course, the difficulty that twenty-four-hour urine sample is acquired when prior art detection is avoided.
Description
Technical field
The present invention relates to clinical medicines to examine field, and in particular to a kind of graphene brilliant cresyl blue urinary albumin test electricity
The production method of pole.
Background technique
Urinary albumin is nephrosis early stage important sensitive indicator.It is also the angiosises such as kidney caused by diabetes, hypertension
Degenerative disease non-invasive monitoring goldstandard.Have become a great public health problem of China or even the whole world in recent decades,
The disease incidence of chronic kidney disease is worldwide in growth trend, 1.3 hundred million people of Patients with Chronic Kidney Disease in China year by year, be after
The another major disease for directly threatening human health after cardiovascular and cerebrovascular disease, diabetes, tumour.
But during present clinical medicine is examined, urinary albumin is examined and mostly uses enzyme-linked immunization, radioimmunology, efficiently greatly
Liquid chromatography and immunoturbidimetry.Wherein:
Enzyme-linked immunization detection time is longer；Radioimmunology sensitivity, accuracy are higher, but there are radioactivity dirts
Dye.
High performance liquid chromatography complex disposal process, operating process are cumbersome.
Immune scatter turbidimetry is the method that current clinical examination commonly measures urinary albumin, due to urinary albumin content
Very low (normal value is less than 20mg/L), the sensibility and specificity of Immune scatter turbidimetry can not all measure the accurate of urinary albumin
Value, therefore testing result cannot function as the foundation of Accurate Diagnosis kidney injury, and checkout procedure takes a long time, from patient's specimen taken
It is needed 4~5 hours to inspection result is obtained about, is unable to satisfy modernization precisely the easy, quick of medical treatment, Accurate Diagnosis and monitoring disease
The requirement of disease.
Summary of the invention
In order to realize rapid, the accuracy, high sensitivity of urinary albumin detection, it is an object of the invention to: provide one
The production method of kind graphene brilliant cresyl blue urinary albumin test electrode.
To achieve the above object, the invention provides the following technical scheme:
A kind of production method of graphene brilliant cresyl blue urinary albumin test electrode, comprising the following steps:
(1) it the preparation of pet substrate: directly buys；
(2) production of graphene working electrode:
(2.1) graphene working electrode is by 85-95 DEG C under hydrothermal conditions of dopamine and hydrophilic imidazole ion liquid IL
Isothermal reaction 5-7h, reduction-oxidation type two-dimensional graphene lamella take mutually product with lamella and connect recombination, obtain the three-dimensional of macroscopic view
Porous graphene assembly is then dissolved in water and obtains three-dimensional porous graphene assembling liquid solution；
(2.2) it disperses crosslinking agent in three-dimensional porous graphene assembling liquid solution with inorganic nano array material and obtains
Mixed solution；
(2.3) mixed solution is printed on pet substrate, forms graphene working electrode in 36-38 DEG C of drying；
(5) production of reference electrode:
Reference electrode is silver/silver chloride electrode, the production method is as follows: PET will be printed in after silver/silver chloride solution dissolution
Substrate surface；
(6) to the production of electrode:
It is carbon electrode to electrode, the production method is as follows: pet substrate surface is printed in after carbon solution is dissolved；
(5) production of insulating layer
It uses print process that polymer insulation paint is printed in except insertion end and reaction zone are with the pet substrate of exterior domain, is formed
Insulating layer, wherein the graphene working electrode, reference electrode are insertion end to the region where electrode leading portion, described
Graphene working electrode, reference electrode are reaction zone to the region where electrode back segment；
(6) production of graphene brilliant cresyl blue urinary albumin test electrode:
By crosslinking agent and urinary albumin selective reaction object solution, graphene work electricity is spread evenly across in the method for spin coating
Pole, silver/silver chlorate, as the sample reaction zone to electrode, are dried, then in reaction zone as reference electrode, carbon in 36-38 DEG C
One layer of PVC insulating film is covered, forms injection port at the edge port of PVC insulating film, it is white to obtain graphene brilliant cresyl blue urine
Albumen test electrode.
Preferably, water, oxidized form two-dimensional graphene nanometer sheet, dopamine and hydrophilic imidazol ion liquid in step (2.1)
The parts by weight of body IL are respectively 15-20 parts, 15-25 parts, 5-15 parts, 45-55 parts.
Preferably, crosslinking agent is naphthols in step (2.2), inorganic nano array material is carboxylic carbon nano-tube；Wherein,
It is respectively 1-5 parts, 20-35 parts, 45- that naphthols, carboxylic carbon nano-tube, three-dimensional porous graphene, which assemble the parts by weight of liquid solution,
60 parts.
Preferably, the length and width of pet substrate, thick respectively 28-30mm, 5.8-6.2mm, 0.7-0.9mm in step (1).
Preferably, the length and width of graphene working electrode, thick respectively 18-22mm, 5.8-6.2mm, 0.3-0.5mm；Reference
The length and width of electrode, thick respectively 18-22mm, 5.8-6.2mm, 0.3-0.5mm；Length and width, thick respectively 18- to electrode
22mm、5.8-6.2mm、0.3-0.5mm。
Preferably, the length and width of insulating layer, thick respectively 18-22mm, 5.8-6.2mm, 0.3-0.5mm in step (5).
Preferably, crosslinking agent is naphthols in step (6), and urinary albumin selective reaction object is brilliant cresyl blue；Water, naphthalene
Phenol, brilliant cresyl blue parts by weight be respectively 85-95 parts, 1-5 parts, 5-15 parts.
Preferably, the length and width of PVC insulating film, thick respectively 5-6mm, 1.5-2.5mm, 0.05-0.15mm in step (6).
Compared with prior art, the beneficial effects of the present invention are:
1) its electric conductivity is fabulous by using graphene working electrode by the present invention, and the electric current generated when detection is made almost
Reach zero loss, ensure that the accuracy of detection；2) reaction of graphene brilliant cresyl blue urinary albumin test electrode of the present invention
Area can be good at avoiding the dry of other visible components in urine by urinary albumin selective reaction object (brilliant cresyl blue)
It disturbs, and selective reaction object (brilliant cresyl blue) reaction sensitivity is very high, is capable of detecting when the urinary albumin of extremely low concentration, greatly
The accuracy of low concentration urinary albumin is improved greatly；3) when graphene brilliant cresyl blue urinary albumin test electrode detection of the present invention
It is to generate curent change by albumin reaction in urinary albumin selective reaction object (brilliant cresyl blue) and urine to obtain detection
As a result, therefore, having time-consuming short, greatly improving work efficiency；In addition, can accomplish the content for detecting urinary albumin in due course,
Avoid the difficulty that twenty-four-hour urine sample is acquired when prior art detection.
Detailed description of the invention
Fig. 1 is that the structure for the graphene brilliant cresyl blue urinary albumin test electrode that better embodiment of the present invention provides is shown
It is intended to.
Fig. 2 is the side structure schematic diagram that graphene brilliant cresyl blue urinary albumin of the present invention tests electrode.
In appended drawing reference: 10-PET substrate, tri- electrode of 20-, 21- graphene working electrode, 22- reference electrode, 23- are to electricity
Pole, 30- insulating layer, 40-PVC insulating film, 41- injection port, 50- reaction zone.
Specific embodiment
In order to make the objectives, technical solutions, and advantages of the present invention clearer, with reference to the accompanying drawings and embodiments, right
The present invention is further elaborated.It should be appreciated that the specific embodiments described herein are merely illustrative of the present invention, and
It is not used in the restriction present invention.
The production method of graphene brilliant cresyl blue urinary albumin test electrode of the present invention, comprising the following steps:
1, the preparation of pet substrate: pet substrate is outsourcing part, and preferred size is 30mm x 6mm x0.8mm.
2, the production of three electrodes: three electrodes are respectively working electrode, reference electrode and the production to electrode.
1) production of working electrode: the graphene working electrode is by reducing agent dopamine (parts by weight 10%) and hydrophilic miaow
Oxazolinium ion liquid IL (parts by weight 50%) (1-Butyl-3-methylimidazolium tetrafluoroborate,
BMIMBF4) 90 DEG C isothermal reaction 6 hours under hydrothermal conditions, reduction-oxidation type two-dimensional graphene (parts by weight 20%) lamella with
Lamella takes mutually product and connection recombination, and it is porous to construct macroscopic three dimensional using oxidized form two-dimensional graphene nanometer sheet as structural unit
Graphene assembly, then by by crosslinking agent (naphthols) (parts by weight 3%) and inorganic nano array material (carboxylated carbon nanometer
Pipe) (parts by weight 30%) be scattered in three-dimensional porous graphene (parts by weight 60%) assembling liquid solution in, by nano material and stone
Synergistic effect between black alkene increases the electricity between electrode active surface site and electrode adsorption ability, promotion electrode and analyte
Son transmitting, the graphene assembling liquid solution for accelerating electrochemical reaction speed, the electrocatalysis characteristic for improving electrode；Then using printing
Method mixes three-dimensional porous graphene assembly, crosslinking agent (naphthols) with inorganic nano array material (carboxylic carbon nano-tube)
Solution is printed in pet substrate, forms graphene working electrode in 37 DEG C of drying.
2) production of reference electrode: reference electrode is silver/silver chloride electrode, and silver/silver chlorate is that commercially available analysis is pure.After dissolution
It is printed in pet substrate surface.It is preferred that printed dimensions are 20mm x 0.9mm x 0.3mm.
3) to the production of electrode: being carbon electrode to electrode.Carbon is commercially available activated carbon, and pet substrate surface is printed in after dissolution.
It is preferred that printed dimensions are 20mm x 0.9mm x 0.3mm.
3, use print process that polymer insulation paint is printed in except insertion end and reaction zone are with the pet substrate of exterior domain, shape
At insulating film, insulated paint is commercially available.It is preferred that printed dimensions are 20mm x 6mm x 0.4mm.
4, the rhetorical functionization in electrode reaction area is made graphene brilliant cresyl blue urinary albumin and tests electrode: crosslinking agent
(naphthols) (parts by weight 3%) and urinary albumin selective reaction object (brilliant cresyl blue) solution (parts by weight 10%), with spin coating
Method is spread evenly across graphene working electrode, silver/silver chlorate as reference electrode, carbon as the sample reaction zone to electrode
Domain is dried in 37 DEG C, is then covered one layer of PVC insulating layer cover film in reaction zone and is formed injection port, and graphene brilliance is obtained
Cresyl blue urinary albumin tests electrode.PVC insulating layer cover film preferred size is 5.5mm x 2.0mm x 0.1mm.
Graphene brilliant cresyl blue urinary albumin test electrode of the present invention is current medical test circle in Analysis of urine albumin head
The secondary research field into electrochemical test.
Principle of products: the electrode is inserted on Electrochemical Detection platform, platform gives electrode one constant voltage, makes electricity
Stream flows through working electrode and constitutes a system that is obstructed or being powered less substantially to electrode, working electrode and reference electrode, utilizes
The stability of reference electrode current potential measures the electrode potential of working electrode.Working electrode and the body that an energization is constituted to electrode
System, for measuring the electric current that working electrode passes through.By urine to be measured close to the well of electrode, electrode is automatically complete by siphon
Electrode reaction area, the urinary albumin selective substances of reaction zone are tested at quantitative suction sample to graphene brilliant cresyl blue urinary albumin
Brilliant cresyl blue is reacted with the albumin in urine, so as to cause electricity in original working electrode and the system being powered to electrode
The variation of stream, and the size of curent change is directly proportional to albumin content in urine, it is big to read curent change by electrochemistry platform
It is small, it is compared automatically with before test with the current curve figure that the urinary albumin calibration object of known concentration is drawn, it is white to calculate urine
Protein content.
The present invention realizes clinical examination completion detection quick when urinary albumin is examined, in due course, accurate, is that other show
There is detection method incomparable.
Experimental result:
6 batches are taken to be purchased from the microdose urine protein quality-control product of the different known concentrations of Britain's Landau production, respectively with exempting from
Epidemic disease turbidimetry and graphene brilliant cresyl blue urinary albumin of the invention test electrode are tested.
Instrument: Shanghai Chen Hua CHI600E electrochemical analyser, 7600 Biochemical Analyzer of Hitachi
Reagent: graceful microdose urine protein assay kit (immunoturbidimetry) lot number in Neusoft Witter
MLB1705023
Method: 6 batch microdose urine protein quality-control products graphene brilliant cresyl blue provided by the invention is urinated respectively
Albumin tests electrode in the graceful microdose urine protein assay kit of Shanghai Chen Hua CHI600E electrochemical analyser and Neusoft Witter
(immunoturbidimetry) is tested on 7600 Biochemical Analyzer of Hitachi, and each batch is tested 3 times respectively.
Conclusion: the test result of graphene brilliant cresyl blue urinary albumin test electrode of the present invention is very close to Quality Control target
Value, and the test result of immunoturbidimetry deviates Quality Control target value.Above experiments have shown that graphene brilliant cresyl blue of the invention is urinated
Albumin test electrode can accurately detect urinary albumin content.
The foregoing is merely illustrative of the preferred embodiments of the present invention, is not intended to limit the invention, all in essence of the invention
Made any modifications, equivalent replacements, and improvements etc., should all be included in the protection scope of the present invention within mind and principle.
Claims (8)
1. a kind of production method of graphene brilliant cresyl blue urinary albumin test electrode, it is characterised in that: the following steps are included:
(1) it the preparation of pet substrate: directly buys；
(2) production of graphene working electrode:
(2.1) graphene working electrode is by dopamine and hydrophilic imidazole ion liquid IL 85-95 DEG C of constant temperature under hydrothermal conditions
5-7h is reacted, reduction-oxidation type two-dimensional graphene lamella takes mutually product with lamella and connect recombination, obtains the three-dimensional porous of macroscopic view
Graphene assembly, be then dissolved in water and obtain three-dimensional porous graphene assembling liquid solution；
(2.2) it disperses crosslinking agent in three-dimensional porous graphene assembling liquid solution with inorganic nano array material and is mixed
Solution；
(2.3) mixed solution is printed on pet substrate, forms graphene working electrode in 36-38 DEG C of drying；
(3) production of reference electrode:
Reference electrode is silver/silver chloride electrode, the production method is as follows: pet substrate will be printed in after silver/silver chloride solution dissolution
Surface；
(4) to the production of electrode:
It is carbon electrode to electrode, the production method is as follows: pet substrate surface is printed in after carbon solution is dissolved；
(5) production of insulating layer
It uses print process that polymer insulation paint is printed in except insertion end and reaction zone are with the pet substrate of exterior domain, forms insulation
Layer, wherein the graphene working electrode, reference electrode are insertion end, the graphite to the region where electrode leading portion
Alkene working electrode, reference electrode are reaction zone to the region where electrode back segment；
(6) production of graphene brilliant cresyl blue urinary albumin test electrode:
By crosslinking agent and urinary albumin selective reaction object solution, with the method for spin coating be spread evenly across graphene working electrode,
Silver/silver chlorate, as the sample reaction zone to electrode, is dried as reference electrode, carbon in 36-38 DEG C, is then covered in reaction zone
One layer of PVC insulating film forms injection port at the edge port of PVC insulating film, obtains graphene brilliant cresyl blue urinary albumin
Test electrode.
2. the production method of graphene brilliant cresyl blue urinary albumin test electrode according to claim 1, feature exist
In: the parts by weight of water, oxidized form two-dimensional graphene nanometer sheet, dopamine and hydrophilic imidazole ion liquid IL in step (2.1)
Respectively 15-20 parts, 15-25 parts, 5-15 parts, 45-55 parts.
3. the production method of graphene brilliant cresyl blue urinary albumin test electrode according to claim 1, feature exist
In: crosslinking agent is naphthols, inorganic nano array material is carboxylic carbon nano-tube in step (2.2)；Wherein, naphthols, carboxylated
Carbon nanotube, the parts by weight of three-dimensional porous graphene assembling liquid solution are respectively 1-5 parts, 20-35 parts, 45-60 parts.
4. the production method of graphene brilliant cresyl blue urinary albumin test electrode according to claim 1, feature exist
In: the length and width of pet substrate, thick respectively 28-30mm, 5.8-6.2mm, 0.7-0.9mm in step (1).
5. the production method of graphene brilliant cresyl blue urinary albumin test electrode according to claim 1, feature exist
In: length and width, thick respectively 18-22mm, 5.8-6.2mm, 0.3-0.5mm of graphene working electrode；The length and width of reference electrode,
Thickness is respectively 18-22mm, 5.8-6.2mm, 0.3-0.5mm；To the length and width of electrode, it is thick be respectively 18-22mm, 5.8-6.2mm,
0.3-0.5mm。
6. the production method of graphene brilliant cresyl blue urinary albumin test electrode according to claim 1, feature exist
In: the length and width of insulating layer, thick respectively 18-22mm, 5.8-6.2mm, 0.3-0.5mm in step (5).
7. the production method of graphene brilliant cresyl blue urinary albumin test electrode according to claim 1, feature exist
In: crosslinking agent is naphthols in step (6), and urinary albumin selective reaction object is brilliant cresyl blue；Water, naphthols, brilliant cresyl blue
Parts by weight be respectively 85-95 parts, 1-5 parts, 5-15 parts.
8. the production method of graphene brilliant cresyl blue urinary albumin test electrode according to claim 1, feature exist
In: the length and width of PVC insulating film, thick respectively 5-6mm, 1.5-2.5mm, 0.05-0.15mm in step (6).
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110487865A (en) * | 2019-09-04 | 2019-11-22 | 安徽信灵检验医学科技股份有限公司 | A kind of production method of urinary albumin test electrode |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110487865A (en) * | 2019-09-04 | 2019-11-22 | 安徽信灵检验医学科技股份有限公司 | A kind of production method of urinary albumin test electrode |
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Application publication date: 20190308 |