CN106093166A - Based on material with carbon element for electrode detecting nicotine and its preparation method and application - Google Patents
Based on material with carbon element for electrode detecting nicotine and its preparation method and application Download PDFInfo
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- CN106093166A CN106093166A CN201610402632.XA CN201610402632A CN106093166A CN 106093166 A CN106093166 A CN 106093166A CN 201610402632 A CN201610402632 A CN 201610402632A CN 106093166 A CN106093166 A CN 106093166A
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- G01N27/30—Electrodes, e.g. test electrodes; Half-cells
- G01N27/308—Electrodes, e.g. test electrodes; Half-cells at least partially made of carbon
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Abstract
The present invention provides a kind of electrode for detecting nicotine based on material with carbon element and its preparation method and application, and its preparation method includes: material with carbon element is purified by (1)；(2) modified electrode: utilize the material with carbon element in described step (1) to modify basal electrode, uses electrode of the present invention to can be used for detecting nicotine, before testing without pretreatment nicotine, highly sensitive, has the strongest market application foreground.
Description
Technical field
The present invention relates to a kind of electrode and preparation method thereof, particularly relate to a kind of based on material with carbon element ancient for detecting Buddhist nun
Electrode of fourth and its preparation method and application.
Background technology
Nicotine is a kind of amine substance being made up of pyridine ring and pyrrole ring, is the alkaloid that in Nicotiana tabacum L., content is most.
Having at present the medicated cigarette of various different brands on the market, wherein the content of Nicotine in Tobacco is one and judges cigarette quality
Index.Additionally, nicotine has certain drug value for treating some brain diseasess, people can be stimulated mainly due to nicotine
The nervus centralis of class brain so that it is produce excited sensation.Therefore, detection nicotine has great value.
The main method being usually used in detecting nicotine at present has spectrophotography, chromatography, immunological method.Although these
Nicotine can be measured by method accurately, but these methods need complicated preprocessing process, needs cost the longest
Time, moreover, the instrument used by detection is costly, and needs professional to operate on it.This is the most greatly
Hinder the universal of nicotine detecting instrument.Meanwhile, the instrument build used by these detection methods is big, and detection environmental requirement is tight
Lattice, are difficult to detect nicotine in real time.
At present, material with carbon element is a kind of modified electrode material being widely used in and preparing electrode, and common material with carbon element has space zero
The carbon nano-cluster of dimension structure, the CNT of space one-dimentional structure, the Graphene of space two-dimensional structure and the stone of Heteroatom doping
Ink alkene, CNT.They have a characteristic of some nano materials: skin effect, quantum size effect, small-size effect and grand
See quantum path effect etc..Skin effect refer to the atomic number of material surface and the ratio of total atom number with particle diameter diminish and drastically
Increase, thus cause qualitative change.Cause the ligancy of atom not enough increasing of carbon material surface atomic number, have
Undersaturated key and many defects and be in an unsure state, in order to reach stable state, easily tie with other atom
Closing or occur the transfer of some electronics, this makes the electron transfer capacity height of material with carbon element, has good electric conductivity and electrochemistry
Performance.The form that in the most different material with carbon elements, carbon atom exists is different, their electric property also can difference, some
Nitrogen, sulfur, waits heteroatomic doping, can change the Electronic Performance of material with carbon element originally, thus promote its chemical property.
Summary of the invention
The shortcoming of prior art in view of the above, it is an object of the invention to provide a kind of convenient, fast and efficient
Based on material with carbon element for electrode detecting nicotine and preparation method thereof.
For achieving the above object and other relevant purposes, the invention provides a kind of based on material with carbon element ancient for detecting Buddhist nun
The preparation method of the electrode of fourth, described preparation method at least includes:
(1) material with carbon element is purified；
(2) modified electrode: utilize the material with carbon element in described step (1) to modify basal electrode.
Preferably, any one or a few in graphite, CNT or carbon fiber of material with carbon element in described step (1)
Mixing.
Preferably, the method that in described step (1), purification uses is any one in acid wash, hydrogen peroxide oxidation process
Or both are used in combination.
It is highly preferred that the acid that described acid wash uses is inorganic strong protonic acid.
It is highly preferred that: described inorganic strong protonic acid is selected from referring to that one or more appointed in sulphuric acid, nitric acid, phosphoric acid are mixed
Close.
Preferably, being slowly added dropwise strong oxidizer while described pickling, mixed solution is stirred heating, described is strong
Oxidant refers to the one in potassium permanganate or potassium hyperchlorate.
Preferably, the concentration of described material with carbon element is 0.1-3mg/mL, and described modified electrode refers to drip on basal electrode 1
～the material with carbon element of 10uL.
Preferably, described step (1) also includes carrying out material with carbon element after purification functionalization, and described functionalization refers to use
One or more use in conjunction in covalent bonding, non-covalent bonding or doping.
Preferably, any one or the two kinds of associatings during described functionalization refers to electrochemical reducing or chemical reduction method
Application.
Preferably, described chemical reduction method is gone back original reagent in ammonia, sodium borohydride, ascorbic acid or hydrazine hydrate
Any one or several use in conjunction.
Preferably, described basal electrode is selected from glass electrode, screen printing electrode, carbon paste electrode, ito glass electrode, gold
In electrode or graphite electrode one or more.
It is highly preferred that described screen printing electrode needs pretreated before modification, described pretreatment specifically refer to
Screen printing electrode, as electrolyte solution, is scanned by the sulphuric acid of 0.5-1mol/L by cyclic voltammetry, removes surface
Impurity.
Another aspect of the present invention there is provided a kind of electrode, and described electrode is adopted and prepared with the aforedescribed process.
Another aspect of the present invention there is provided the method using above-mentioned electrode, and it is ancient that described electrode is used for detecting Buddhist nun
Fourth.
As it has been described above, the present invention based on material with carbon element for the electrode detecting nicotine and preparation method thereof, have with
Lower beneficial effect:
(1) due to the characteristic that nicotine is oxidizable, when Electrochemical Detection, when applied voltage reaches its oxidizing potential, Buddhist nun
Ancient fourth will lose electronics generation oxidation reaction at electrode surface, and electrode will capture electronics, and it be migrated rapidly, it is thus achieved that letter
Number.This needs exist for good electrical property, and the many material of avtive spot is modified on the surface of electrode, therefore, with material with carbon element prepare for
The electrode sensitivity of nicotine detection is high, response time is short, good stability, reproducible；
(2) electrode detection nicotine of the present invention is without carrying out pretreatment to nicotine, the shortest, convenient,
It is prone to carry out the dynamic tracing detection of nicotine, is a kind of with a high credibility and modern detecting accurately.
Accompanying drawing explanation
Transmission electron microscope figure (TEM) figure of the nitrogen-doped graphene material that Fig. 1 is prepared by embodiment 1；
X-ray photoelectron power spectrum (XPS) figure of the nitrogen-doped graphene material that Fig. 2 is prepared by embodiment 1；
Fig. 3 is by embodiment, electrochemical AC impedance (EIS) figure of the Different electrodes of 1 preparation；
The modified electrode that Fig. 4 is prepared by embodiment 2 cyclic voltammetric qualitative to nicotine (CV) figure；
The modified electrode that Fig. 5 is prepared by embodiment 2 responds (I-t) curve to nicotine chrono-amperometric；
The modified electrode that Fig. 6 is prepared by embodiment 2 responds reproducible test result to nicotine；
The modified electrode that Fig. 7 is prepared by embodiment 2 responds selective test result to nicotine.
Detailed description of the invention
Below by way of specific instantiation, embodiments of the present invention being described, those skilled in the art can be by this specification
Disclosed content understands other advantages and effect of the present invention easily.The present invention can also be by the most different concrete realities
The mode of executing is carried out or applies, the every details in this specification can also based on different viewpoints and application, without departing from
Various modification or change is carried out under the spirit of the present invention.It should be clear that the process equipment specifically not indicated in the following example or device
All use the conventional equipment in this area or device.In addition, it is to be understood that the one or more method steps mentioned in the present invention are also
Do not repel and can also there is additive method step before and after described combination step or also may be used between these steps specifically mentioned
To insert additive method step, except as otherwise noted；Should also be understood that one or more equipment/devices of mentioning in the present invention it
Between combination annexation do not repel and can also there are other equipment/devices before and after described unit equipment/device or at this
Other equipment/devices can also be inserted, except as otherwise noted between two the equipment/devices specifically mentioned a bit.And, unless separately
Being described, the numbering of various method steps is only the convenient tool differentiating various method steps, rather than for limit the row of various method steps
Row order or the restriction enforceable scope of the present invention, being altered or modified of its relativeness, without essence change technology contents
In the case of, when being also considered as the enforceable category of the present invention.
Embodiment 1 utilizes the screen printing electrode preparation method of graphene modified
Material with carbon element is purified and functionalization by step (1)
Graphene is purified by a: weighs 3.0g Graphene and is dissolved in the concentrated sulphuric acid (360mL) of volume ratio is 9:1 98%
With in 98% strong phosphoric acid (40mL) mixed solution, it is slowly added to the potassium permanganate solution of 6%wt, mixed solution is heated to 50
DEG C, constant temperature stirring 12h, to take out, room temperature cools down.The hydrogenperoxide steam generator of 30% (v/v) of 3mL is added again in above-mentioned solution,
Ice bath.The product hydrochloric acid and the ultra-pure water that take out respectively are washed 3 times, are then vacuum dried.
B is by graphene functionalized after purification: taking above-mentioned dried graphene oxide 0.1g, ultrasonic dissolution is in 108mL
2%wt ammonia spirit in, stirring, be heated to 80 DEG C, react 6h.Cooling, with milli-Q water 3～5 times, 35 DEG C of vacuum are done
Dry 12h.Obtain the Graphene of nitrating.This material carrying out TEM and XPS characterize, such as Fig. 1 and 2, result shows, nitrogen-doped graphene
There is Graphene thin-walled layer, the shape characteristic such as fold.From the result of XPS, nitrogen element is successfully doped to graphene-structured
In, content is 7.64%.
Step (2) precondition substrate electrode
Using the screen printing carbon electrode of preparation as working electrode, with platinum electrode, silver/silver chloride electrode constitutes three electrode systems
System, CV scanning 40 circle in the sulfuric acid solution of 0.5mol/L (it is of course also possible to selecting 0.6-1mol/L's), voltage range is
1.5～2.0V.Electrode after activation is cleaned with ultra-pure water, the most stand-by.Measure the electrochemical AC impedance of Different electrodes
(EIS), its result is as shown in Figure 3.
Step (3) prepares modified electrode
The nitrogen-doped graphene synthesized by step (1) and water are configured to the solution of 0.1-3mg/mL (for example, it may be 1mg/
ML), take 10 these solution of μ L to drop on processed screen printing carbon electrode, it is also possible to take 1-6 μ L, be added drop-wise on electrode, room
Temperature is dried, and obtains required electrode.
Embodiment 2 utilizes the electrode in embodiment 1 to detect nicotine
(1) qualitative detection of nicotine
With the phosphate buffer solution (PBS, PH=7.4) of 0.1mol/L as electrolyte, the basal electrode of preparation is as work
Making electrode, it is carried out CV scanning, then add the nicotine solution of 50 μ L1mg/mL in this solution, stirring, identical
Under the conditions of, carry out CV scanning (such as Fig. 4) again.By comparing the result of CV curve, it is known that, nicotine occurs on this electrode
Oxidation, and oxidation current is produced when current potential is 0.6V.
(2) detection by quantitative of nicotine
Using chronoamperometry (I-t) that nicotine is carried out detection by quantitative, voltage is set to 0.85V.At uniform stirring
The solution of 5mL PBS (PH=7.4) adds the nicotine solution of 40 μ L 1mg/mL every 50s, until reaching saturation.
By IT curve (such as Fig. 5), after adding nicotine, electrode can provide response rapidly.Meanwhile, by processing IT curve,
Can calculate this electrode to the range of linearity of nicotine is 0-200 μm ol/L, 250-500 μM.Sensitivity reaches 0.626mA
Cm-2mmol-1L, lowest detection is limited to 0.04723 μm ol/L.
(3) the repeatability detection of nicotine
Using chronoamperometry (I-t) that nicotine is carried out detection by quantitative, voltage is set to 0.85V.Select basal signal
Identical six roots of sensation basal electrode, modifies with nitrogen-doped graphene material.5mL PBS (PH=7.4) molten at uniform stirring
Liquid adds the nicotine solution of 20 μ L 1mg/mL every 50s.Repeat six experiments.Such as Fig. 6, experimental result understands, adds
Entering same concentration nicotine, between electrode, response difference is less, and its relative standard deviation is 1.4%.Therefore, this electrode is to nicotine
Response there is good repeatability.
(4) nicotine anti-interference detection
Using chronoamperometry (I-t) that nicotine is carried out detection by quantitative, voltage is set to 0.85V.At uniform stirring
The solution of 5mL PBS (PH=7.4) is separately added into the nicotine solution of 25 μm ol/L, the Vitamin C of 25 μm ol/L every 50s
Acid (AA) and the uric acid (UA) of 1mmol/L, glucose (GLu), iron chloride, calcium chloride, potassium chloride and ammonium chloride solution.Such as Fig. 7,
Can be obtained by result, interference material is on this electrode almost without response, and the detection on nicotine does not affect.Therefore this electrode
Nicotine is had good selectivity.
Embodiment 3 utilizes the preparation method of carbon nano tube modified screen printing electrode
Material with carbon element is purified and functionalization by step (1)
The CNT taking 1g adds concentrated nitric acid and concentrated sulphuric acid condensing reflux at 80 DEG C of 30mL89% of 30mL 65%
Reacted product is carried out washing to solution as neutral by 2h., and the product obtained after filtration is standby after vacuum drying.
Step (2) precondition substrate electrode
Using the screen printing carbon electrode of preparation as working electrode, with platinum electrode, silver/silver chloride electrode constitutes three electrode systems
System, CV scanning 40 circle in the sulfuric acid solution of 0.5mol/L, voltage range is 1.5～2.0V.By the electrode after activation with ultrapure
Water cleans, the most stand-by.
Step (3) prepares modified electrode
The CNT synthesized by step (1) and water are configured to the solution of (0.1-2) mg/mL (for example, it is possible to make 0.5mg/
ML), take 10 these solution of μ L and drop on processed screen printing carbon electrode, drying at room temperature, obtain required electrode.Certainly,
5-9 μ L can also be taken be added drop-wise on electrode.
Certainly, those skilled in the art all understands, in the particular embodiment, according to the difference of the material with carbon element being selected from,
Any one or both that the mode of its functionalization is also further selected from electrochemical reducing or chemical reduction method are used in combination,
If again with chemical reduction method, then going back original reagent and can be selected from ammonia, selected from ammonia, sodium borohydride, ascorbic acid or hydrazine hydrate
In one or more use in conjunction.
The above, only presently preferred embodiments of the present invention, not any formal and substantial to present invention restriction,
It should be pointed out that, for those skilled in the art, on the premise of without departing from the inventive method, also can make
Some improvement and supplement, these improve and supplement also should be regarded as protection scope of the present invention.All those skilled in the art,
Without departing from the spirit and scope of the present invention, make when available disclosed above technology contents a little more
The equivalent variations moved, modify and develop, is the Equivalent embodiments of the present invention；Meanwhile, all substantial technological pair according to the present invention
The change of any equivalent variations that above-described embodiment is made, modify and develop, all still fall within the scope of technical scheme
In.
Claims (14)
1. the preparation method of the electrode for detecting nicotine based on material with carbon element, it is characterised in that described preparation method
At least include:
(1) material with carbon element is purified；
(2) modified electrode: utilize the material with carbon element in described step (1) to modify basal electrode.
The preparation method of the electrode for detecting nicotine based on material with carbon element the most according to claim 1, its feature exists
In: material with carbon element any one or a few mixing in graphite, CNT or carbon fiber in described step (1).
The preparation method of the electrode for detecting nicotine based on material with carbon element the most according to claim 1, its feature exists
In: the method that in described step (1), purification uses is any one or both associatings in acid wash, hydrogen peroxide oxidation process
Use.
The preparation method of the electrode for detecting nicotine based on material with carbon element the most according to claim 3, its feature exists
In: the acid that described acid wash uses is inorganic strong protonic acid.
The preparation method of the electrode for detecting nicotine based on material with carbon element the most according to claim 4, its feature exists
In: described inorganic strong protonic acid is selected from referring to that one or more appointed in sulphuric acid, nitric acid, phosphoric acid mix.
The preparation method of the electrode for detecting nicotine based on material with carbon element the most according to claim 5, its feature exists
In: being slowly added dropwise strong oxidizer while described pickling, mixed solution is stirred heating, described strong oxidizer refers to height
One in potassium manganate or potassium hyperchlorate.
The preparation method of the electrode for detecting nicotine based on material with carbon element the most according to claim 1, its feature exists
In: the concentration of described material with carbon element is 0.1-3mg/mL, and described modified electrode refers to drip the carbon material of 1～10uL on basal electrode
Material.
The preparation method of the electrode for detecting nicotine based on material with carbon element the most according to claim 1, its feature exists
In: described step (1) also includes carrying out material with carbon element after purification functionalization, and described functionalization refers to use covalent bonding, non-
One or more use in conjunction in covalent bonding or doping.
The preparation method of the electrode for detecting nicotine based on material with carbon element the most according to claim 1, its feature exists
Any one or two kinds of use in conjunction in electrochemical reducing or chemical reduction method are referred in: described functionalization.
The preparation method of the electrode for detecting nicotine based on material with carbon element the most according to claim 9, its feature exists
In: described chemical reduction method is gone back original reagent in ammonia, sodium borohydride, ascorbic acid or hydrazine hydrate any one or
Several use in conjunction.
The preparation method of 11. electrodes for detecting nicotine based on material with carbon element according to claim 1, its feature exists
In: described basal electrode is selected from glass electrode, screen printing electrode, carbon paste electrode, ito glass electrode, gold electrode or graphite electricity
In extremely one or more.
The preparation method of 12. electrodes for detecting nicotine based on material with carbon element according to claim 11, its feature
Being: described screen printing electrode needs pretreated before modification, described pretreatment specifically refers to the sulfur with 0.5-1mol/L
Screen printing electrode, as electrolyte solution, is scanned by acid by cyclic voltammetry, removes the impurity on surface.
13. 1 kinds of electrodes, it is characterised in that: described electrode uses the method system described in claim 1-12 any claim
Standby.
14. electrodes as claimed in claim 13 are used for detecting nicotine.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111505097A (en) * | 2020-06-12 | 2020-08-07 | 上海烟草集团有限责任公司 | Electrochemical method for measuring nicotine content in tobacco and tobacco related products |
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