CN220251808U - Portable plasticizer analysis device and detection system based on electrochemical sensor - Google Patents
Portable plasticizer analysis device and detection system based on electrochemical sensor Download PDFInfo
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- Investigating Or Analysing Biological Materials (AREA)
Abstract
The utility model provides a portable plasticizer analysis device and a detection system based on an electrochemical sensor, wherein the analysis device is connected with an electric sensor for specifically adsorbing phthalate plasticizers, analyzes the phthalate plasticizers and displays the results, and the portable plasticizer analysis device comprises a shell, an electric sensor socket arranged at one side end of the shell, an analysis electrode electrically connected with the electric sensor socket, a data storage chip, a signal converter, a microprocessor, a display screen and a power supply. When the electrochemical sensor is inserted into the socket and then connected with the analysis electrode, the device is automatically started, then electrolyte is dripped into the detection pool, the microprocessor acquires the peak current of the working electrode in the analysis electrode, converts an electrochemical signal into a concentration value according to a standard curve in the data storage chip, and then displays the concentration information on the display screen through the signal converter.
Description
Technical Field
The utility model belongs to the technical field of plasticizer detection, and provides a portable plasticizer analysis device and a detection system based on a phthalate plasticizer electrochemical sensor.
Background
Phthalate (PAEs) plasticizers are widely used to increase the flexibility and ductility of products such as plastic packaging, but have chemical structures similar to our human female hormone, interfere with normal hormone levels after entering the human body, and are at some risk of carcinogenesis. PAEs have been classified as tightly controlled contaminants in countries around the world, a range of standard regulations have been established, and there are clear requirements for specific migration limits of PAEs in food-contact materials. The national food safety national Standard food contact Material and additive use Standard for articles (GB 9685-2016) standardizes the regulatory execution standards for PAEs, wherein the specific migration amounts of diisononyl phthalate (DINP), di-n-butyl phthalate (DBP) and other phthalate plasticizers are 9.0mg/kg, 0.3mg/kg and 1.5mg/kg respectively. Therefore, detection and monitoring of the low-dose plasticizer in the food are carried out, so that the harm to human health is reduced, and the method is a necessary measure for improving the safety of environmental food.
At present, large-scale instruments such as liquid chromatography, mass spectrometry and the like are generally adopted for detecting PAEs plasticizers, but sample pretreatment is troublesome, and the detection process is long in time consumption, so that the detection result is delayed from the production quality control requirement. Therefore, there is a need to develop a portable device for fast and convenient PAEs for fast detection and monitoring of low-dose plasticizers in foods on site.
Electrochemical detection is a high-efficiency method for detecting the relationship between the electrochemical property (such as current) of a substance to be detected and the concentration change thereof, for example, detecting the blood glucose index in blood based on electrochemical sensing, and detecting the environmental formaldehyde content in an electrochemical sensor formaldehyde detection device CN 207908420U. Because of simple and convenient instrument operation and high sensitivity, the method is widely applied to the fields of food processing, pharmaceutical engineering, environment detection and the like. Therefore, the developed electric sensor modified by the plasticizer molecular imprinting material is combined, the portable equipment which is simple to operate, reliable in performance and capable of rapidly detecting small electrochemical sensing detection on site is developed, and the portable equipment has important practical value for research in the fields of food safety detection, environment detection and the like.
Disclosure of Invention
The utility model provides a portable plasticizer analysis device based on a plasticizer molecular imprinting electric sensor, which is matched with an electric sensor of phthalate plasticizers, analyzes and displays detection results, and is used for rapidly detecting phthalate plasticizers in the fields of food safety detection, environmental protection and the like.
According to a first aspect of the utility model, there is provided a portable plasticizer analysis device based on an electrochemical sensor, connected to an electrical sensor that specifically adsorbs phthalate plasticizers, for analyzing and displaying the results, comprising a housing, an electrical sensor socket disposed at one side of the housing, an analysis electrode electrically connected to the electrical sensor socket, a data storage chip, a signal converter, a microprocessor, a display screen, and a power source.
The analysis electrode comprises a working electrode, a reference electrode and a counter electrode, and a detection pool for supplying power to the liquid drop is arranged above the working electrode; the data storage chip is electrically connected with the analysis electrode, and a quantitative relation standard curve between the concentration of the reference solution and the electric signal is stored.
The device of the utility model takes the target plasticizer molecules to be detected as reference substances, establishes the quantitative relation of the chemical sensing signal reference substance concentration, and then carries out qualitative analysis on the plasticizer molecules with unknown concentration. When the electrochemical sensor is inserted into the socket and then connected with the analysis electrode, the device is automatically started, then electrolyte is dripped into the detection pool, the microprocessor acquires the peak current of the working electrode in the analysis electrode, converts an electrochemical signal into a concentration value according to a standard curve in the data storage chip, and then displays the concentration information on the display screen through the signal converter.
Preferably, the shell is rectangular and comprises a bottom cover and an upper end cover, and the electric sensor socket is arranged at the foremost end of the shell;
one end of the analysis electrode is electrically connected with the electric sensor socket, and the other end of the analysis electrode is electrically connected with the data storage chip. The analysis electrode also comprises a constant voltage single chip, provides constant voltage required by test, and keeps stable electrode potential of the three-electrode system in the working process.
The signal converter is an I/C signal converter, and is led into the device through the chip, and when the sample is detected, the device automatically reports the concentration value of the detected sample according to the concentration and the change of I current; the microprocessor is an MCU microprocessor.
The display screen is an active matrix LCD, and mainly uses current to stimulate liquid crystal molecules to generate points, lines and surfaces, and the points, lines and surfaces are matched with back lamps to form a picture.
The data storage chip is purchased in the market, is connected with the data converter in the box body, and is a chip for storing the linear relation between the concentration and the signal in advance.
The display screen is arranged on the shell, the power supply is connected with the display screen, the I/C signal converter, the memory and the like, and the single machine controller is connected with the power supply.
In a second aspect of the utility model, a phthalate plasticizer detection system is provided, comprising an electrical sensor that specifically adsorbs phthalate plasticizers, and an analysis device electrically connected to the electrical sensor and analyzing the same.
The analysis device is the portable plasticizer analysis device.
The electric sensor comprises a working electrode, a reference electrode and a counter electrode. The surface of the working electrode is modified with imprinted polymer X-MIP based on phthalate plasticizer molecules, the imprinted polymer X-MIP is prepared by performing free radical bulk polymerization on target phthalate plasticizer molecules X, polymer monomers, an initiator and a cross-linking agent respectively, eluting by adopting a mixed solvent of methanol and acetic acid, and drying in vacuum.
Preferably, X is selected from any one of the following formulas 1 to 16:
preferably, the polymer monomer is selected from any one of methacrylic acid, 2-vinyl pyridine, 2-vinyl thiophene and 4-vinyl pyridine; the initiator is azobisisobutyronitrile, and the cross-linking agent is ethylene glycol dimethacrylate.
Preferably, when free radical polymerization is carried out, the polymerization temperature is 60-80 ℃ and the polymerization time is 6-24 hours; during elution, the volume ratio of the methanol to the acetic acid solution is 9:1, and the elution time is 1-48 h; the vacuum drying temperature is 65-80 ℃ and the drying time is 12-48 h.
The preparation method of the electric sensor comprises the following steps:
1) Immersing the screen printing electrode into sulfuric acid or hydrochloric acid solution with the concentration of 0.1mol/L for cyclic voltammetry scanning activation; uniformly mixing the molecularly imprinted polymer X-MIP with chitosan solution by ultrasonic to form slurry, coating the polymer slurry on a pretreated screen printing electrode by adopting a drop coating method, and naturally airing at room temperature to obtain a working electrode of the molecularly imprinted polymer X-MIP loaded with PAEs plasticizer;
2) And (3) correctly connecting the working electrode with a reference electrode silver/silver chloride electrode and a counter electrode platinum electrode to obtain the electric sensor.
In a third aspect of the present utility model, a method for rapidly detecting phthalate plasticizers by using the phthalate plasticizer detection system is provided, comprising the following steps:
1) Extracting a sample to be detected by a compound extraction liquid to obtain a pretreatment liquid, inserting an electric sensor for specifically adsorbing phthalate plasticizers into the pretreatment extraction liquid, incubating for 10min, taking out, and naturally airing;
2) Then the electric sensor is inserted into an electric sensor socket of the analysis device and connected with an analysis electrode in the device, the module is automatically started, and then a certain amount of potassium ferricyanide electrolyte is dripped into a detection pool to start detection; the microprocessor acquires peak current of a working electrode in the analysis electrode, converts an electrochemical signal into a concentration value according to a standard curve in the data storage chip, and then displays concentration information on a display screen through a signal converter.
Preferably, in the step 1), the compound extract is a mixed solution of acetonitrile and n-hexane with the volume ratio of 20:1, the compound extract and a sample to be tested are mixed for ultrasonic treatment for 20min, and the supernatant is sucked and collected to be used as a sample pretreatment solution; in step 2), the amount of potassium ferricyanide electrolyte added was 20. Mu.L.
The beneficial effects of the utility model are as follows:
in the preparation aspect, the imprinted polymer X-MIP for carrying out working electrode modification is prepared by carrying out free radical bulk polymerization on target phthalate plasticizer molecules X, a polymer monomer, an initiator and a cross-linking agent respectively, eluting by adopting a mixed solvent of methanol and acetic acid, and carrying out vacuum drying. When the PAEs plasticizer loaded molecularly imprinted polymer X-MIP is loaded on a working electrode, the working electrode loaded on the PAEs plasticizer molecularly imprinted polymer X-MIP can be obtained by immersing the screen printed electrode in 0.1mol/L sulfuric acid or hydrochloric acid solution for cyclic voltammetry scanning activation, then uniformly mixing the molecularly imprinted polymer X-MIP with chitosan solution by ultrasound to form slurry, coating the slurry on the pretreated screen printed electrode, and naturally airing at room temperature. The preparation of the imprinted polymer X-MIP, the working electrode and the electric sensor has the advantages of few reagent types, mild process conditions, simple post-treatment, low cost and easy realization;
the analysis device comprises a shell, an electric sensor socket arranged at one side end of the shell, an analysis electrode electrically connected with the electric sensor socket, a data storage chip, a signal converter, a microprocessor, a display screen and a power supply, and has the beneficial effects of miniaturization, targeting, high sensitivity, convenience in operation, low price and the like.
In the aspect of effect, the electrochemical sensor based on the molecularly imprinted polymer prepared by the utility model is used for detecting PAEs plasticizer, and has the advantages of quick response, high selectivity, high sensitivity, field detection and the like. The complex pretreatment process of the sample is avoided, the operation procedure is simplified, the detection cost is reduced, and the detection channel is widened.
Through practical verification, the electrochemical sensor based on the molecularly imprinted polymer prepared by the utility model has lower minimum detection limit on 16 PAEs plasticizers in edible oil, and the minimum detection limit of certain substances is far lower than the national standard.
Drawings
FIG. 1 is a schematic diagram of a portable plasticizer analyzer;
FIG. 2 is a schematic structural diagram of an electrical sensor that specifically adsorbs phthalate plasticizers;
fig. 3 is a schematic flow chart of a main program of a working system of the plasticizer inspection apparatus.
Detailed Description
The present utility model will be described in detail with reference to the drawings and examples thereof, which are provided on the premise of the technical solution of the present utility model, and the detailed embodiments and specific operation procedures are given, but the scope of the present utility model is not limited to the following examples.
For a better understanding of the present utility model, and not to limit its scope, all numbers expressing quantities, percentages, and other values used in the present application are to be understood as being modified in all instances by the term "about". Accordingly, unless indicated otherwise, the numerical parameters set forth in the specification and attached claims are approximations that may vary depending upon the desired properties sought to be obtained. Each numerical parameter should at least be construed in light of the number of reported significant digits and by applying ordinary rounding techniques.
Example 1
The portable plasticizer analysis device 100 (fig. 1) based on the electrochemical sensor of this embodiment is connected to the electric sensor 200 (fig. 2) that specifically adsorbs phthalate plasticizers, and analyzes it and displays the result. The portable plasticizer analysis device 100 based on the electrochemical sensor comprises a shell 1, an electric sensor socket 2, an analysis electrode 3, a data storage chip 4, a signal converter 5, a microprocessor 6, a display screen 7, a power supply 8 and a connecting wire 9.
The shell 1 is rectangular and comprises a bottom cover and an upper end cover; the electric sensor socket 2 is arranged at the forefront end of the shell and is used for installing an electric sensor 200 for specifically adsorbing phthalate plasticizers; one end of the analysis electrode 3 is electrically connected with the electric sensor socket 2, and the other end is electrically connected with the data storage chip 4; the microprocessor 6 is arranged in the middle of the shell 1, and the signal converter 5, the display screen 7 and the power supply 8 are arranged in the rear half section of the shell, so that the microprocessor 6 is conveniently connected with all components in the shell.
The analysis electrode 3 is a three-electrode system and comprises a working electrode, a reference electrode and a counter electrode, and a detection pool for supplying power to the liquid drop is arranged above the working electrode; the three-electrode system also comprises a constant voltage single chip, which provides a constant voltage required by the test and keeps stable electrode potential in the working process.
The data storage chip 4 is electrically connected with the analysis electrode, and a quantitative relation standard curve between the concentration of the reference solution and the electric signal is stored. The built-in I-C linear relationship is the linear relationship between signal value and concentration as detected from a plasticizer/acetonitrile solution of known concentration. The test is carried out in advance and is led into the I/C converter through the memory chip, and when a sample is detected, the device can automatically convert data according to the test value and display the data on a display screen.
The signal converter 5 is an I/C signal converter and is led into the device through a chip; the microprocessor 6 is an MCU microprocessor; the display screen 7 is an active matrix liquid crystal display, and mainly uses current to stimulate liquid crystal molecules to generate points, lines and surfaces which are matched with back lamp tubes to form a picture; the power supply 8 is connected with the display screen, the I/C signal converter, the memory and the like.
The analysis device takes target plasticizer molecules to be detected as reference substances, establishes quantitative relation of chemical sensing signal reference substance concentration, and performs qualitative analysis on plasticizer molecules with unknown concentration. When the electrochemical sensor is inserted into the socket and then connected with the analysis electrode, the device is automatically started, then electrolyte is dripped into the detection pool, the microprocessor acquires the peak current of the working electrode in the analysis electrode, converts an electrochemical signal into a concentration value according to a standard curve in the data storage chip, and then displays the concentration information on the display screen through the signal converter, so that quick response and detection of the plasticizer are realized.
The structure of an electrical sensor 200 that specifically adsorbs phthalate plasticizers is shown in fig. 2, which is also a three-electrode system, including a working electrode, a reference electrode, and a counter electrode. The surface of the working electrode is modified with imprinted polymer X-MIP based on phthalate plasticizer molecules, the imprinted polymer X-MIP is prepared by performing free radical bulk polymerization on target phthalate plasticizer molecules X, polymer monomers, an initiator and a cross-linking agent respectively, eluting by adopting a mixed solvent of methanol and acetic acid, and drying in vacuum.
The electric sensor is prepared by adopting a screen printing technology, and the method comprises the following steps:
1) Immersing the screen printing electrode into sulfuric acid or hydrochloric acid solution with the concentration of 0.1mol/L for cyclic voltammetry scanning activation; uniformly mixing the molecularly imprinted polymer X-MIP with chitosan solution by ultrasonic to form slurry, coating the polymer slurry on a pretreated screen printing electrode by adopting a drop coating method, and naturally airing at room temperature to obtain a working electrode of the molecularly imprinted polymer X-MIP loaded with PAEs plasticizer;
2) And (3) correctly connecting the working electrode with a reference electrode silver/silver chloride electrode and a counter electrode platinum electrode to obtain the electric sensor.
During detection, firstly, extracting a sample to be detected by a compound extraction liquid to obtain a pretreatment liquid, then inserting an electric sensor 200 for specifically adsorbing phthalate plasticizers into the pretreatment extraction liquid for incubation for 10min, taking out and naturally airing; the electric sensor is then plugged into an electric sensor socket of the analysis device, connected with an analysis electrode in the device, and the analysis device analyzes and displays the detection result.
The specific process of data analysis using the analysis device is shown in fig. 3, and is as follows:
firstly, the power supply 8 is turned ON to enable the display screen to display a normal state, the microprocessor 6 controls the device to self-diagnose the electrode, and the normal state is broadcast through the voice reminder 10, and the display screen displays an ON state. Inserting an electric sensor 200 which is adsorbed with the specific phthalate plasticizer of the sample to be detected into an electric sensor socket 2 and electrically connecting with an analysis electrode 3; after the electrolyte potassium ferricyanide is dripped, analysis is automatically started, a microprocessor obtains peak current of a working electrode in an analysis electrode, an electric signal is automatically converted into concentration information according to a standard curve in a data storage chip 4, then the MCU microprocessor sorts, stores and transmits the collected concentration information into an I/C signal converter 5, the I/C signal converter 5 records and outputs the converted concentration information, finally the concentration information is displayed on a display screen 7, the concentration value of a sample to be tested is broadcasted through voice, and the sample test is finished. The power is turned OFF and the display 7 displays the OFF state.
While the preferred embodiments of the present utility model have been illustrated and described, the present utility model is not limited to the embodiments, and various equivalent modifications and substitutions can be made by one skilled in the art without departing from the spirit of the present utility model, and these equivalent modifications and substitutions are intended to be included in the scope of the present utility model as defined in the appended claims.
Claims (7)
1. A portable plasticizer analyzer based on an electrochemical sensor, connected to an electrical sensor that specifically adsorbs phthalate plasticizers, for analysis and display of the results, comprising:
the shell, the electric sensor socket arranged at one side end of the shell, the analysis electrode electrically connected with the electric sensor socket, the data storage chip, the signal converter, the microprocessor, the display screen and the power supply,
the analysis electrode comprises a working electrode, a reference electrode and a counter electrode, and a detection pool for supplying power to the liquid drop is arranged above the working electrode; the data storage chip is electrically connected with the analysis electrode, and a quantitative relation standard curve between the concentration of the reference solution and the electric signal is stored in the data storage chip.
2. The electrochemical-sensor-based portable plasticizer analysis device of claim 1, wherein:
the shell is rectangular and comprises a bottom cover and an upper end cover, and the electric sensor socket is arranged at the forefront end of the shell.
3. The electrochemical-sensor-based portable plasticizer analysis device of claim 1, wherein:
one end of the analysis electrode is electrically connected with the electric sensor socket, and the other end of the analysis electrode is electrically connected with the data storage chip.
4. The electrochemical-sensor-based portable plasticizer analysis device of claim 1, wherein:
the analysis electrode also comprises a constant voltage single chip, provides constant voltage required by test, and keeps stable electrode potential of the three-electrode system in the working process.
5. The electrochemical-sensor-based portable plasticizer analysis device of claim 1, wherein:
wherein the signal converter is an I/C signal converter; the microprocessor is an MCU microprocessor; the display screen is an active matrix liquid crystal display.
6. The electrochemical-sensor-based portable plasticizer analysis device of claim 1, wherein:
the electric sensor comprises a working electrode, a reference electrode and a counter electrode, wherein the surface of the working electrode is modified with imprinted polymer based on phthalate plasticizer molecules.
7. A portable plasticizer detection system based on an electrochemical sensor is characterized by comprising an electric sensor for specifically adsorbing phthalate plasticizers and an analysis device electrically connected with the electric sensor and used for analyzing the electric sensor,
wherein the electric sensor comprises a working electrode, a reference electrode and a counter electrode, the surface of the working electrode is modified with imprinted polymer based on phthalate plasticizer molecules,
the analyzer according to any one of claims 1 to 6.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN202320303020.0U CN220251808U (en) | 2023-02-24 | 2023-02-24 | Portable plasticizer analysis device and detection system based on electrochemical sensor |
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| Application Number | Priority Date | Filing Date | Title |
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| CN202320303020.0U CN220251808U (en) | 2023-02-24 | 2023-02-24 | Portable plasticizer analysis device and detection system based on electrochemical sensor |
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