CN113109412A - Portable field nicotine detection method based on gold nanoparticle modified screen-printed electrode - Google Patents
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Abstract
The invention provides a portable on-site nicotine detection method based on a gold nanoparticle modified screen-printed electrode, which creatively selects an electrochemical regulation method, simplifies the crystal face regulation step, reduces the cost, simultaneously realizes the direct exposure of the crystal face of a gold electrode, ensures that the gold electrode generates good selective response to nicotine, drips the prepared detection liquid onto the obtained gold nanoparticle modified SPE electrode, and fits a continuous curve according to the equivalent voltage and current obtained in official software PSTrace of an intelligent nicotine detection platform and the specific current-nicotine content value, thereby being convenient for the calculation of nicotine content; the CV method determination and standard curve fitting processes are packaged into a small program algorithm, so that the nicotine measurement value is rapidly displayed in a 'field detection' module; the process of converting the current value to a nicotine content value is encapsulated in a preprogrammed algorithm so that the nicotine detection value can be displayed in real time in the applet.
Description
Technical Field
The invention belongs to the technical field of nicotine detection, and particularly relates to a portable field nicotine detection method based on a gold nanoparticle modified screen-printed electrode.
Background
In the last two decades, researchers developed many methods for measuring nicotine, such as spectrophotometry, liquid chromatography, high performance liquid chromatography-electrochemical (HPLC-EC), gas chromatography-mass spectrometry (GC-MS), titration, gravimetric methods, Atomic Absorption Spectrophotometry (AAS), etc., and electrochemical methods have been increasingly used for qualitative and quantitative detection of nicotine due to their remarkable characteristics of high sensitivity, fast response, simple operation, less sample requirement, portability, low price, and capability of realizing on-site on-line detection and analysis. The Emstat electrochemical workstation has the characteristic of being portable, has the function of visualizing current and other data with the PSTrace software, but lacks the functions of content report and the like required to be generated in the aspect of nicotine detection.
Chinese patent CN103630461B discloses a portable field detection nicotine system based on gold nanoparticle (Au PN) modified SPE electrode, which includes gold nanoparticle modified Screen Printing (SPE) electrode, portable electrochemical workstation Emstat and "niguchi fast detection" small program and its data cloud platform. The invention adopts the technology of the electrochemical interface construction based on the regulation and control of the crystal face of Au and the rapid detection of nicotine in a complex sample, and the technology regulates and controls the crystal face exposure of the surface of an Au electrode by a simple electrochemical method to construct a high-sensitivity and high-selectivity electrochemical interface, thereby generating specific response to the nicotine in the complex sample and realizing the selective detection of the nicotine. Meanwhile, by combining with a passive sampler and other kits, through the processes of sample collection, sample pretreatment, sample detection and data processing and combining with a small program 'Niguy quick test', a visual report of the nicotine content level in tobacco, environmental medium and human body is obtained.
Disclosure of Invention
Aiming at the defects, the invention provides a portable on-site nicotine detection method based on the gold nanoparticle modified silk-screen printing electrode prepared by an electrochemical regulation and control method.
The invention provides the following technical scheme: the portable field nicotine detection method based on the gold nanoparticle modified screen-printed electrode comprises the following steps:
1) preparing a gold nanoparticle modified silk-screen printing electrode: sucking octahedral gold nanoparticles and dripping the octahedral gold nanoparticles on the surface of a screen-printed electrode, and drying the octahedral gold nanoparticles for 24 hours at 25 ℃ to obtain the gold nanoparticle modified screen-printed electrode;
2) after the pretreatment of the sample is finished, dropping the prepared detection liquid onto the SPE electrode modified by the gold nanoparticles obtained in the step 1), and installing the electrode at the specified position of the portable electrochemical workstation Emstat to perform electrochemical detection; drawing a standard curve according to the equivalent values of voltage and current obtained in official software PSTrace of an intelligent nicotine detection platform, and fitting a continuous curve according to the specific current-nicotine content value, so that the nicotine content can be conveniently obtained; the CV method determination and standard curve fitting processes are packaged into a small program algorithm, so that the nicotine measurement value is rapidly displayed in a 'field detection' module;
3) the process of converting the current value to a nicotine content value is encapsulated in a preprogrammed algorithm so that the nicotine detection value can be displayed in real time in the applet.
Further, the continuous curve equation in step 2) is: y-a-bln (x + c), where y is the current in μ a and x is the concentration in μ g/g.
Further, the intelligent nicotine detection platform comprises a Bluetooth connection module, a data processing module, a cloud data storage module and a detection report visualization module. The Nichu quick detection small program in the attached drawing of the invention is an intelligent nicotine detection platform, and the nicotine database is a cloud data storage module.
Further, the monitoring records generated by the intelligent nicotine detection platform include daily reports, weekly reports, monthly reports, and annual reports.
Further, the data stored by the cloud data storage module of the intelligent nicotine detection platform comprises basic information, physical and chemical properties, tobacco addiction and nicotine content in cigarettes.
Further, the nicotine detected by the method comprises tobacco, air and urine.
The invention has the beneficial effects that:
1. the invention innovatively selects an electrochemical regulation method, simplifies the crystal face regulation step, reduces the cost, and simultaneously realizes the direct exposure of the crystal face of the Au electrode surface (111), so that the Au electrode surface has good selective response to nicotine.
3. Portability and miniaturization: the collection of air nicotine is realized by combining the electrochemical sensor with the passive sampler. The passive sampler is portable and miniaturized, can track the activities of people, is used for monitoring the individual contact quantity evaluation, and can also be placed in a place to be tested for continuous sampling and used for indoor air quality evaluation and monitoring. The nicotine rapid detector is installed in a public place, and the Internet of things is formed, so that real-time data can be provided for governments, and the establishment of a smoking control policy is assisted.
4. High sensitivity: the electrochemical sensor has the characteristics of high sensitivity and high efficiency. The octahedral gold nanoparticle AuNP is physically modified on the surface of an Au electrode and subjected to surface pretreatment, so that the response of the electrode to nicotine is remarkably improved, and the detection effect is superior to that of the original common electrode. By comparison, the CV method selected by the product is more sensitive to nicotine detection than other electrochemical analysis methods, and the linear range is 10-200 mug/g.
5. Universality: on the basis of a portable simple field detector, a portable simple field detection intelligent system based on SPE electrodes (screen printing electrodes) is created by combining a single chip microcomputer, various peripheral devices, mobile phone applets, a database and the like, the system comprises the detector and software equipment, a software part in the system becomes a universal component by methods such as cloud computing and data api opening, and the system can be rapidly applied to scenes with different requirements and serves as one of components in various projects.
6. Networking and intelligentization:
the intellectualization is embodied as follows: the small program end comprises the functions of detection guidance, data analysis, result visualization report display, historical data query comparison and the like. The detection equipment is integrated, the microprocessor and the Bluetooth module are combined, instant wireless transmission of data in the detection process is achieved, and visual display of required curves and charts is carried out through the built-in data processing module.
The networking is embodied in: the small program records the detection result every time and uploads the detection result to the cloud, a huge nicotine detection information database is formed, data api is opened, and other projects or application calling are facilitated. Or the module of the invention is directly applied and matched with other external software and hardware modules, thereby widening the application field. For example, the nicotine detection of tobacco leaves is increased to be applied to the tobacco industry; increasing blood nicotine detection for medical applications; air nicotine detection is added for application in the environmental monitoring industry.
Drawings
The invention will be described in more detail hereinafter on the basis of embodiments and with reference to the accompanying drawings. Wherein:
FIG. 1 is a general flow diagram of a method for detecting nicotine provided by the present invention;
FIG. 2 is a TEM image of gold nanoparticles employed for modifying screen-printed electrodes according to the invention:
in the figure: (a) spherical; (b) a cube; (c) an octahedron; (d) a cube; (e) an octahedron;
FIG. 3 is a schematic diagram of the effect of detecting 100 μ g/g nicotine by using a spherical, cubic, octahedral gold nanoparticle modified screen printed electrode and a common screen printed electrode provided by the present invention;
fig. 4 is a CV graph (left) and a fitting curve graph (right) of standard nicotine samples with different concentrations measured by the nicotine detection method provided by the invention;
FIG. 5 is a CV diagram (left) and a histogram (right) of nicotine measured at different pH values according to the nicotine detection method provided by the present invention;
fig. 6 is a functional explanatory diagram of an intelligent nicotine detection platform, namely a niguo quick detection small program, adopted by the nicotine detection method provided by the invention.
Detailed description of the preferred embodiments
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The method for obtaining three detection samples as shown in fig. 1 comprises the following steps: taking a certain amount of tobacco samples when detecting nicotine in tobacco leaves; when detecting nicotine in the air, wearing the passive individual sampler at the pocket of the coat or placing the passive individual sampler at a place to be detected, and continuously sampling for 8-24 h; to detect nicotine in a medical sample, the subject's urine or blood, etc. is collected in a numbered sample bottle. The pretreatment of the sample should also be determined according to the type of sample to be tested:
(1) determination of nicotine content in tobacco samples (solids)
a. Weighing 20mg of tobacco powder (200mg of tobacco), adding 4mL of hydrochloric acid (HCl) to dissolve out nicotine in the tobacco powder (tobacco), and shaking for 3 minutes;
b. after the oscillation is finished, obtaining a brownish yellow clear liquid through film coating;
(2) determination of nicotine content in air (gas)
Sampling by using a passive sampler containing activated carbon, taking out the activated carbon adsorption layer after sampling, and eluting by using carbon disulfide to obtain a solution;
(3) determination of nicotine content in urine (liquid)
Adding a proper amount of NaOH solution into a sampling bottle for alkalization;
after the pretreatment of the sample is finished, 2mL of solution is taken, 2mL of PBS buffer solution is added according to the proportion of 1:1 to form detection solution, then the detection solution is dropped on the SPE electrode modified by the gold nanoparticles, and the electrode is installed at the specified position of the portable electrochemical workstation Emstat to carry out electrochemical detection.
Here, gold nanoparticle modified SPE electrodes are explained with reference to fig. 2.
Experiments prove that different crystal faces of Au play an important role in the electrocatalytic performance of nicotine, and the Au (111) crystal face (namely the exposed crystal face of the octahedron gold nanoparticle (AuNP)) has the best electrocatalytic activity on nicotine, so that the gold crystal face can be further exposed through electrochemical regulation and control treatment. The preparation method of the gold nanoparticle modified SPE electrode comprises the following steps: and sucking 50 mu L of octahedral AuNP, dropwise adding the octahedral AuNP on the surface of the SPE electrode, drying at 25 ℃ for 24 hours, and then carrying out electrochemical regulation treatment to obtain the octahedral AuNP modified SPE electrode.
And (3) detecting the performance of the gold nanoparticle modified SPE electrode by adopting nicotine standard solutions with different concentrations:
taking 10 mu L, 20 mu L, 40 mu L, 60 mu L, 80 mu L, 100 mu L, 120 mu L, 140 mu L, 160 mu L, 180 mu L and 200 mu L of the nicotine standard solution, respectively, adding the nicotine standard solution into 1mL of 1% acetic acid, considering that the nicotine content unit in the actual tobacco is mu g/g and the density of the nicotine and the acetic acid is 1g/mL, directly converting the concentration into mu g/g to obtain the standard solutions of 10 mu g/g, 20 mu g/g, 40 mu g/g, 60 mu g/g, 80 mu g/g, 100 mu g/g, 120 mu g/g, 140 mu g/g, 160 mu g/g, 180 mu g/g and 200 mu g/g.
120 μ L0.1M H at a measurement voltage of-0.3 to +1.5V by Cyclic Voltammetry (CV) method2SO4And dropwise adding the solution onto an SPE gold electrode for electrochemical treatment, and circulating for 50 circles to obtain a stable circulating voltammogram with the sweep rate of 0.05V. The SPE gold electrode was then carefully washed with ultrapure water and blown dry with air.
Electrochemical behavior characterization of different redox species:
first 120. mu.L of 0.5mM [ Fe (CN)6]3-/4-0.5mM glucose, 0.5mM ascorbic acid solution was dropped on each of the electrochemically conditioned SPEs and electrochemically scanned from 0 to +0.9V by CV method, respectively. The SPE was then washed with ultrapure water and 120. mu.L of a 0.1M H2 SO 4 solution was added dropwise thereto, using Square Wave Voltammetry (SWV) to characterize the electrochemical behavior of such species. Before scanning from +0.8V to a final potential of +1.6V, a voltage is first applied at a conditional potential of-0.2V for 10 s. All scans were performed at a frequency of 10Hz with an amplitude of 25mV and a step voltage of 5 mV.
The Square Wave Voltammetry (SWV) method was chosen to perform 10 consecutive measurements of 100. mu.g/g nicotine. And obtaining stable corresponding parameters of nicotine detection. The following table lists parameters such as the stable response of the working electrode to nicotine detection. The frequency was 10Hz, the amplitude was 25mV, and the step voltage was 5 mV.
The reagents and instruments used were as follows:
1) reagent: octahedral nanogold (10mL, beijing china thundersonics ltd); d-glucose, ascorbic acid, sulfuric acid, potassium ferricyanide, potassium ferrocyanide, potassium dihydrogen phosphate, disodium hydrogen phosphate dodecahydrate, sodium chloride, potassium chloride (analytically pure, national drug group chemical reagents, Inc.); nicotine standards (1000 μ g/g, Sigma, usa); pure water (made by a water purifier).
Wherein the nicotine standard product is prepared by adding nicotine into ultrapure water, and the concentration is 1 g/L. Potassium ferricyanide/potassium ferrocyanide ([ Fe (CN))6]3-/4-) The electrolyte was prepared from 0.5mM potassium ferricyanide, 0.5mM potassium ferrocyanide and 0.1M KCl. Phosphate Buffered Saline (PBS) from 2.0mM KH2PO 4，10.0mM Na 2HPO 4·12H 2O, 136.8mM NaCl and 2.7mM KCl (pH 7.5). All reagents were analytically pure, and solutions were prepared using ultrapure water (resistivity 18 M.OMEGA.cm).
2) The instrument comprises the following steps: DS 220AT screen printed gold electrodes (china ltd, wangton, switzerland); CHI660E square wave voltammetry analysis apparatus (shanghai chenhua instruments ltd).
The electrochemical properties of three AuNPs with different morphologies are characterized. After the surface of the Au electrode is modified by a physical method, nicotine (100 mu g/g) with the same content is respectively measured and compared with a common Au electrode. The result shows that the ordinary Au electrode generates a weaker response to nicotine, the cubic AuNPs lose the original signal due to the introduction of the cubic AuNPs, and the result proves that the (100) surface inhibits the reaction of nicotine on the Au surface, the (111) surface corresponding to the octahedral AuNPs promotes the response of an Au interface to nicotine, and meanwhile, the electrocatalytic activity of the spherical AuNPs with the two crystal surfaces to nicotine is between that of the octahedral AuNPs and that of the cubic AuNPs, and the effect of the spherical AuNPs is superior to that of the ordinary Au electrode. The above results demonstrate that the different crystal planes of Au play an important role in the electrocatalytic properties of nicotine, and that the Au (111) crystal plane has the best electrocatalytic activity for nicotine.
For the modified electrode with the gold (111) crystal face, the electrode is known to have strong response to nicotine, and 100 mug/g is measured continuously by Square Wave Voltammetry (SWV), so that stable electrochemical response parameters are obtained finally. A linear response in the range of 10. mu.g/g to 200. mu.g/g concentration was obtained.
The current-voltage relationship graph and the like after electrochemical detection can be obtained in the official software PSTrace distributed by Emstat.
The nicotine standard solution with the same concentration is selected and tested in PBS buffer solution under different pH conditions. The experiment result shows that the electrode has the best effect of detecting nicotine when the pH value is 8, so that PBS buffer solution with the pH value of 8 is adopted in the follow-up process. (FIG. 4)
Taking the measurement of nicotine content in an actual tobacco sample as an example, under the scheme of sample pretreatment, nicotine standard solutions with different concentrations are added into hydrochloric acid, a 1:1 solution and a 0.01mol/L PBS solution with pH of 8 are mixed, CV method measurement is carried out, the voltage is 0-0.9V, and the sweep rate is 0.05V/s (figure 5). Fitting was performed using the equation y-a-bln (x + c) (where y is the current (μ a) and x is the concentration (μ g/g)), as follows:
the results show that the electrode has a good linear relation for detecting nicotine in a certain range, and the fitted curve is that y is-2.652 +0.423ln (x +584.06), R2Linear range 15-400 μ g/g ═ 0.993. The linear range of the method can cover the nicotine content in the actual sample with reference to the nicotine content in the actual sample.
The CV method measurements and the standard curve fitting process are packaged into a small programmed algorithm for rapid display of nicotine measurements in the "in situ test" module. As shown in fig. 6, the small program is divided into three parts of field detection, nicotine database and monitoring record: the first step of the ' on-site detection ' is ' device connection ', detection abandon ' or ' device connection ' can be selected, the former is clicked to return to a main interface, the latter is clicked to start judging whether the system Bluetooth connection is successful, the next step is continued, the no step is returned to the first step and prompt hardware debugging, and the second step is sample information filling, including sample number filling, sample quality filling and the like. If the electrode is put into the solution, the detection can be started, the detection result, namely the nicotine content taking mu g/g as the unit, is displayed after a few seconds, the algorithm of the step is the cyclic voltammetry and the standard curve fitting, and finally the detection result is put into a nicotine database.
The monitoring record mainly monitors the nicotine intake of smokers in real time to form a daily report, a weekly report, a monthly report and an annual report, thereby achieving the purpose of controlling the smoking. The nicotine database is divided into several blocks of basic information, physical and chemical properties, tobacco addiction and nicotine content in cigarette, and serves the purposes of popularization and historical measurement data retrieval.
Gold nanoparticle modified SPE electrode: the SPE electrode is an Emstat matched electrode, and the detection effect is improved after the gold nanoparticles are modified.
The portable electrochemical workstation Emstat and the matched PSTrace software thereof: and mounting the modified SPE electrode to Emstat, and reading the values of the measured current and voltage in the PSTrace.
The small program of the 'Niugu quick test' and the data cloud platform thereof are as follows: packaging a current-nicotine content conversion method, namely a CV method and curve fitting, into a fixed algorithm, and realizing real-time display of a detection result by matching with hardware; meanwhile, the cloud database stores historical detection data and other huge data used for science popularization.
The above embodiments are only used to illustrate the technical solution of the present invention, and not to limit the same; while the invention has been described in detail and with reference to the foregoing embodiments, it will be understood by those skilled in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some or all of the technical features may be equivalently replaced; and the modifications or the substitutions do not make the essence of the corresponding technical solutions depart from the scope of the technical solutions of the embodiments of the present invention.
Furthermore, those skilled in the art will appreciate that while some embodiments herein include some features included in other embodiments, rather than other features, combinations of features of different embodiments are meant to be within the scope of the invention and form different embodiments. For example, in the claims above, any of the claimed embodiments may be used in any combination. The information disclosed in this background section is only for enhancement of understanding of the general background of the invention and should not be taken as an acknowledgement or any form of suggestion that this information forms the prior art already known to a person skilled in the art.
Claims (6)
1. The portable field nicotine detection method based on the gold nanoparticle modified screen-printed electrode is characterized by comprising the following steps:
1) preparing a gold nanoparticle modified silk-screen printing electrode: sucking octahedral gold nanoparticles and dripping the octahedral gold nanoparticles on the surface of a screen-printed electrode, and drying the octahedral gold nanoparticles for 24 hours at 25 ℃ to obtain the gold nanoparticle modified screen-printed electrode;
2) after the pretreatment of the sample is finished, dropping the prepared detection liquid onto the SPE electrode modified by the gold nanoparticles obtained in the step 1), and installing the electrode at the specified position of the portable electrochemical workstation Emstat to perform electrochemical detection; drawing a standard curve according to the equivalent values of voltage and current obtained in official software PSTrace of an intelligent nicotine detection platform, and fitting a continuous curve according to the specific current-nicotine content value, so that the nicotine content can be conveniently obtained; the CV method determination and standard curve fitting processes are packaged into a small program algorithm, so that the nicotine measurement value is rapidly displayed in a 'field detection' module;
3) the process of converting the current value to a nicotine content value is encapsulated in a preprogrammed algorithm so that the nicotine detection value can be displayed in real time in the applet.
2. The portable field nicotine detection method based on gold nanoparticle modified screen-printed electrodes according to claim 1, wherein the continuous curve equation in step 2) is as follows: y-a-bln (x + c), where y is the current in μ a and x is the concentration in μ g/g.
3. The portable field detection nicotine method based on gold nanoparticle modified screen-printed electrodes of claim 1, wherein the intelligent nicotine detection platform comprises a bluetooth connection module, a data processing module, a cloud data storage module and a detection report visualization module.
4. The portable field nicotine detection method based on gold nanoparticle modified screen printed electrodes according to claim 1, wherein the monitoring records generated by the intelligent nicotine detection platform comprise daily reports, weekly reports, monthly reports and annual reports.
5. The portable field detection nicotine method based on gold nanoparticle modified screen-printed electrodes of claim 1, wherein the data stored by the cloud data storage module of the intelligent nicotine detection platform comprises basic information, physicochemical properties, tobacco addiction and nicotine content in cigarettes.
6. The method for portable field detection of nicotine based on gold nanoparticle modified screen printed electrodes as claimed in claim 1, wherein the nicotine detected by the method comprises tobacco, air and urine.
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