CN115047055B - Method and system for detecting lead ions by sensor - Google Patents
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- CN115047055B CN115047055B CN202210591752.4A CN202210591752A CN115047055B CN 115047055 B CN115047055 B CN 115047055B CN 202210591752 A CN202210591752 A CN 202210591752A CN 115047055 B CN115047055 B CN 115047055B
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- 150000002500 ions Chemical class 0.000 title claims abstract description 40
- 238000000034 method Methods 0.000 title claims abstract description 23
- 238000001514 detection method Methods 0.000 claims abstract description 34
- 108090000790 Enzymes Proteins 0.000 claims abstract description 32
- 102000004190 Enzymes Human genes 0.000 claims abstract description 32
- RVPVRDXYQKGNMQ-UHFFFAOYSA-N lead(2+) Chemical compound [Pb+2] RVPVRDXYQKGNMQ-UHFFFAOYSA-N 0.000 claims abstract description 25
- 239000002096 quantum dot Substances 0.000 claims abstract description 21
- 239000000758 substrate Substances 0.000 claims abstract description 15
- 230000008859 change Effects 0.000 claims abstract description 12
- 239000008151 electrolyte solution Substances 0.000 claims abstract description 7
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims abstract description 5
- 239000012528 membrane Substances 0.000 claims abstract description 5
- 239000007864 aqueous solution Substances 0.000 claims abstract description 4
- 238000001903 differential pulse voltammetry Methods 0.000 claims abstract description 4
- 238000012937 correction Methods 0.000 claims description 49
- RWSXRVCMGQZWBV-WDSKDSINSA-N glutathione Chemical group OC(=O)[C@@H](N)CCC(=O)N[C@@H](CS)C(=O)NCC(O)=O RWSXRVCMGQZWBV-WDSKDSINSA-N 0.000 claims description 8
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims description 6
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims description 6
- 239000000243 solution Substances 0.000 claims description 5
- 108010024636 Glutathione Proteins 0.000 claims description 4
- 108010001103 Glutathione oxidase Proteins 0.000 claims description 4
- UHYPYGJEEGLRJD-UHFFFAOYSA-N cadmium(2+);selenium(2-) Chemical compound [Se-2].[Cd+2] UHYPYGJEEGLRJD-UHFFFAOYSA-N 0.000 claims description 4
- 229960003180 glutathione Drugs 0.000 claims description 4
- 229910021607 Silver chloride Inorganic materials 0.000 claims description 3
- 229910052697 platinum Inorganic materials 0.000 claims description 3
- 230000008569 process Effects 0.000 claims description 3
- HKZLPVFGJNLROG-UHFFFAOYSA-M silver monochloride Chemical compound [Cl-].[Ag+] HKZLPVFGJNLROG-UHFFFAOYSA-M 0.000 claims description 3
- 239000011780 sodium chloride Substances 0.000 claims description 3
- 238000013519 translation Methods 0.000 claims description 3
- 238000005259 measurement Methods 0.000 claims 2
- 230000000694 effects Effects 0.000 description 4
- 108010000659 Choline oxidase Proteins 0.000 description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N EtOH Substances CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 3
- WQZGKKKJIJFFOK-GASJEMHNSA-N Glucose Natural products OC[C@H]1OC(O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-GASJEMHNSA-N 0.000 description 3
- 108090000854 Oxidoreductases Proteins 0.000 description 3
- 102000004316 Oxidoreductases Human genes 0.000 description 3
- WQZGKKKJIJFFOK-VFUOTHLCSA-N beta-D-glucose Chemical compound OC[C@H]1O[C@@H](O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-VFUOTHLCSA-N 0.000 description 3
- OEYIOHPDSNJKLS-UHFFFAOYSA-N choline Chemical compound C[N+](C)(C)CCO OEYIOHPDSNJKLS-UHFFFAOYSA-N 0.000 description 3
- 229960001231 choline Drugs 0.000 description 3
- 229960001031 glucose Drugs 0.000 description 3
- 239000008103 glucose Substances 0.000 description 3
- 230000009286 beneficial effect Effects 0.000 description 2
- 239000003651 drinking water Substances 0.000 description 2
- 235000020188 drinking water Nutrition 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 230000036541 health Effects 0.000 description 2
- 230000005764 inhibitory process Effects 0.000 description 2
- 238000012544 monitoring process Methods 0.000 description 2
- 238000010791 quenching Methods 0.000 description 2
- 230000000171 quenching effect Effects 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 238000001479 atomic absorption spectroscopy Methods 0.000 description 1
- 238000001391 atomic fluorescence spectroscopy Methods 0.000 description 1
- 210000000133 brain stem Anatomy 0.000 description 1
- 238000000835 electrochemical detection Methods 0.000 description 1
- 239000003344 environmental pollutant Substances 0.000 description 1
- 229910001385 heavy metal Inorganic materials 0.000 description 1
- 238000001095 inductively coupled plasma mass spectrometry Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 210000000653 nervous system Anatomy 0.000 description 1
- 230000008520 organization Effects 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 231100000719 pollutant Toxicity 0.000 description 1
- 238000004416 surface enhanced Raman spectroscopy Methods 0.000 description 1
Classifications
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
- G01N27/26—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating electrochemical variables; by using electrolysis or electrophoresis
- G01N27/416—Systems
- G01N27/48—Systems using polarography, i.e. measuring changes in current under a slowly-varying voltage
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- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Health & Medical Sciences (AREA)
- Physics & Mathematics (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- Molecular Biology (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
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- Investigating Or Analysing Materials By The Use Of Chemical Reactions (AREA)
- Investigating Or Analysing Biological Materials (AREA)
Abstract
The invention discloses a method and a system for detecting lead ions by a sensor, wherein the method comprises the following steps: s1, preparing a sensor for detecting current intensity, wherein the sensor is formed by mixing quantum dots, enzyme and enzyme substrates; s2, dividing the electrolytic cell into a reference area and a detection area by using an alumina membrane electrode, placing a working electrode in the reference area, placing a reference electrode in the detection area, and electrically connecting the working electrode, the reference electrode and an electrochemical workstation to assemble a detection system; and S3, adding electrolyte solution into the reference area and the detection area, applying detection potential to the electrochemical workstation, adding lead ion aqueous solution into the reference area, measuring the change of photocurrent intensity between the reference electrode and the working electrode according to the change of fluorescence intensity of the quantum dots in the sensor, and analyzing the change of photocurrent intensity by adopting a differential pulse voltammetry to obtain a measured value of lead ion concentration so as to realize detection of lead ions. The method for detecting the lead ions accurately and rapidly detects the content of the lead ions.
Description
Technical Field
The invention belongs to the technical field of electrochemical detection, and particularly relates to a method and a system for detecting lead ions by an N sensor.
Background
Heavy metal means that the relative density is 5g/cm 3 The above metals, wherein lead ions are typical. Exceeding the lead ion content in drinking water has important harm to human health, and can cause damage to brain and nervous system in different degrees. The world health organization recommends a safe level of 48nM for lead ion concentration in drinking water. Therefore, it is important to explore a method for sensitively detecting the concentration of lead ions.
The existing detection methods mainly comprise an atomic fluorescence spectrometry, an atomic absorption spectrometry, an inductively coupled plasma mass spectrometry and a surface enhanced Raman spectrometry, but the methods cannot rapidly detect the content of lead ions, are easy to be interfered by the outside, and have large fluctuation of test results.
Disclosure of Invention
The invention mainly solves the technical problem of providing a method and a system for detecting lead ions by using a sensor, which is prepared by adopting quantum dots, enzyme and enzyme substrates, and is based on the inhibition effect of the lead ions on the enzyme activity, so that the quenching degree of the quantum dots is reduced, the current intensity is enhanced, and the content of the lead ions is accurately and rapidly detected.
In order to solve the technical problems, the invention adopts a technical scheme that: a method for detecting lead ions by a sensor, comprising the steps of:
s1, preparing a sensor for detecting current intensity, wherein the sensor is formed by mixing quantum dots, enzyme and enzyme substrates;
s2, placing the sensor in an electrolytic cell, and dividing the electrolytic cell into a reference area and a detection area by using an alumina membrane electrode, wherein the reference area is communicated with the detection area through the sensor; placing a working electrode in a reference area, placing a reference electrode in a detection area, and electrically connecting the working electrode, the reference electrode and an electrochemical workstation to assemble a detection system;
and S3, adding electrolyte solution into the reference area and the detection area, applying detection potential to the electrochemical workstation, adding lead ion aqueous solution into the reference area, measuring the change of photocurrent intensity between a reference electrode and a working electrode according to the change of fluorescence intensity of quantum dots in the sensor, and analyzing the change of photocurrent intensity by adopting a differential pulse voltammetry to obtain a measured value of lead ion concentration so as to realize detection of lead ions.
Further, the detection limit of the lead ion is 0.035nM.
Further, the sensor is made of quantum dots, enzyme and enzyme substrate, wherein the concentration of the quantum dots is 10 -6 ~10 -4 The concentration of the enzyme is 1-8U/mL, and the concentration of the enzyme substrate is 0.5-1 mol/L.
Further, the addition volume ratio of each component in the sensor is 1:0.1:1.
Further, the quantum dot is one of CdSe, cdS or PbS.
Further, the enzyme is one of ethanol oxidase, choline oxidase or glutathione oxidase.
Further, the enzyme substrate is one of glucose, choline or glutathione.
Further, the electrolyte solution is 1mmol/L BaSO 4 Solution or 1mmol/L NaCl solution.
Further, the working electrode is an Ag/AgCl electrode.
Further, the reference electrode is a platinum electrode.
Further, the method for detecting lead ions by the sensor further comprises the following steps:
s4, constructing an error correction library corresponding to the sensor, and correcting the measured value of the lead ion concentration based on the error correction library;
wherein constructing an error correction library corresponding to the sensor comprises:
obtaining a plurality of different first collocations of components mixed to form the sensor, the first collocations comprising: the volume ratio, the type and the concentration of each component;
acquiring a plurality of history error records corresponding to the first collocation scheme;
extracting an error amount in the history error record;
establishing a time axis, and representing the error amount on the time axis based on the record generation time of the history error record corresponding to the error amount;
acquiring a preset trigger frame, translating the trigger frame on the time axis, and calculating a two-to-two subtracted difference value of the error amount falling in the trigger frame each time in the translation process;
based on the error, a trigger index is calculated as follows:
wherein ,for the trigger index, D i D being the i-th difference of the two subtraction of the error amounts falling in the trigger frame 0 For a preset difference threshold, n is the total number of differences, H i Is an intermediate variable;
if the trigger index is greater than or equal to a preset trigger index threshold, calculating an average value of the error amounts falling in the trigger frame;
after the trigger frame translates on the time axis, calculating a first error correction coefficient based on each average value, wherein the calculation formula is as follows:
wherein ,σ1 For the first error correction coefficient, J t For the t-th said average value, Z is the total number of said average values;
pairing the first error correction coefficient with the corresponding first collocation scheme to obtain a pairing item;
constructing an error correction library corresponding to the sensor based on each pairing item;
wherein correcting the measured value of the lead ion concentration based on the error correction library includes:
acquiring a current second collocation scheme of the sensor, and determining a second error correction coefficient corresponding to the second collocation scheme based on the error correction library;
and correcting the measured value of the lead ion concentration based on the second error correction coefficient, wherein a correction formula is as follows:
O′=O+σ 2
wherein O' is the measured value of the concentration of lead ions after correction, O is the measured value of the concentration of lead ions before correction, σ 2 And correcting the coefficient for the second error.
A system for detecting lead ions by using a sensor comprises the sensor, an alumina membrane electrode, an electrolytic cell, a working electrode, a reference electrode and an electrochemical workstation.
The beneficial effects of the invention are at least as follows:
1. the sensor is prepared from the quantum dots, the enzyme and the enzyme substrate, and is based on the inhibition effect of lead ions on the enzyme activity, so that the quenching degree of the quantum dots is reduced, the current intensity is enhanced, and the content of the lead ions is accurately and rapidly detected.
2. The detection method provided by the invention can play an important role in environmental comprehensive control, especially in emergency monitoring of lead ion pollutants and sudden events, and has a wide application prospect in the technical field of environmental monitoring.
Detailed Description
The following detailed description of the preferred embodiments of the invention is provided to enable those skilled in the art to more readily understand the advantages and features of the invention and to make a clear and concise definition of the scope of the invention.
In one embodiment, a method for detecting lead ions by a sensor includes the steps of:
s1, preparing a sensor for detecting current intensity, wherein the sensor is formed by mixing quantum dots, enzyme and enzyme substrates;
s2, placing the sensor in an electrolytic cell, and dividing the electrolytic cell into a reference area and a detection area by using an alumina membrane electrode, wherein the reference area is communicated with the detection area through the sensor; placing a working electrode in a reference area, placing a reference electrode in a detection area, and electrically connecting the working electrode, the reference electrode and an electrochemical workstation to assemble a detection system;
and S3, adding electrolyte solution into the reference area and the detection area, applying detection potential to the electrochemical workstation, adding lead ion aqueous solution into the reference area, measuring the change of photocurrent intensity between a reference electrode and a working electrode according to the change of fluorescence intensity of quantum dots in the sensor, and analyzing the change of photocurrent intensity by adopting a differential pulse voltammetry to obtain a measured value of lead ion concentration so as to realize detection of lead ions.
The detection limit of the lead ions is 0.035nM.
The sensor is made of quantum dots, enzyme and enzyme substrate, wherein the concentration of the quantum dots is 10 -6 ~10 - 4 The concentration of the enzyme is 1-8U/mL, and the concentration of the enzyme substrate is 0.5-1 mol/L.
The addition volume ratio of each component in the sensor is 1:0.1:1.
The quantum dot is one of CdSe, cdS or PbS.
The enzyme is one of ethanol oxidase, choline oxidase or glutathione oxidase.
The enzyme substrate is one of glucose, choline or glutathione.
The electrolyte solution is 1mmol/L BaSO 4 Solution or 1mmol/L NaCl solution.
The working electrode is an Ag/AgCl electrode.
The reference electrode is a platinum electrode.
Examples 1-3 are the components of the sensor of the present invention, and are specifically shown in the following table:
quantum dot (mol/L) | Enzyme (U/mL) | Enzyme substrate (mol/L) | |
Example 1 | CdSe 10 -6 | Ethanol oxidase 1 | Choline 0.5 |
Example 2 | PbS 10 -5 | Choline oxidase 4 | Glucose 0.7 |
Example 3 | CdS 10 -4 | Glutathione oxidase 8 | Glutathione 1 |
The sensor of the present invention was subjected to a correlation performance test with the sensor of the prior art (EG sensor), and the test results were as follows:
sensor for detecting a position of a body | Detection limit (nM) | Object of detection |
Example 1 | 0.035 | Lead ions |
Example 2 | 0.035 | Lead ions |
Example 3 | 0.035 | Lead ions |
EG | 0.053 | Lead ions |
Therefore, the detection limit of the sensor is relatively low, and the sensor is superior to the EG sensor in the prior art.
In one embodiment, a method for detecting lead ions by a sensor further comprises:
s4, constructing an error correction library corresponding to the sensor, and correcting the measured value of the lead ion concentration based on the error correction library;
wherein constructing an error correction library corresponding to the sensor comprises:
obtaining a plurality of different first collocations of components mixed to form the sensor, the first collocations comprising: the volume ratio, the type and the concentration of each component;
acquiring a plurality of history error records corresponding to the first collocation scheme;
extracting an error amount in the history error record;
establishing a time axis, and representing the error amount on the time axis based on the record generation time of the history error record corresponding to the error amount;
acquiring a preset trigger frame, translating the trigger frame on the time axis, and calculating a two-to-two subtracted difference value of the error amount falling in the trigger frame each time in the translation process;
based on the error, a trigger index is calculated as follows:
wherein ,for the trigger index, D i D being the i-th difference of the two subtraction of the error amounts falling in the trigger frame 0 For a preset difference threshold, n is the total number of differences, H i Is an intermediate variable;
if the trigger index is greater than or equal to a preset trigger index threshold, calculating an average value of the error amounts falling in the trigger frame;
after the trigger frame translates on the time axis, calculating a first error correction coefficient based on each average value, wherein the calculation formula is as follows:
wherein ,σ1 For the first error correction coefficient, J t For the t-th said average value, Z is the total number of said average values;
pairing the first error correction coefficient with the corresponding first collocation scheme to obtain a pairing item;
constructing an error correction library corresponding to the sensor based on each pairing item;
wherein correcting the measured value of the lead ion concentration based on the error correction library includes:
acquiring a current second collocation scheme of the sensor, and determining a second error correction coefficient corresponding to the second collocation scheme based on the error correction library;
and correcting the measured value of the lead ion concentration based on the second error correction coefficient, wherein a correction formula is as follows:
O′=O+σ 2
wherein O' is the measured value of the concentration of lead ions after correction, O is the measured value of the concentration of lead ions before correction, σ 2 And correcting the coefficient for the second error.
The working principle and the beneficial effects of the technical scheme are as follows:
because the components of the sensor are mixed and made into different components, the sensor has errors with different degrees when being used for detecting the concentration of lead ions, and in order to further improve the accuracy of the sensor for detecting the concentration of lead ions and the convenience when the sensor is used for detecting the concentration of lead ions, an error correction library corresponding to the sensor needs to be built in advance for error conditions. When a library is constructed, each component mixed to be manufactured into the sensor is matched randomly to obtain a first matching scheme, historical error data of the first matching scheme is obtained, a first error correction coefficient is determined based on the historical error data, and the first error correction coefficient is matched with the corresponding first matching scheme to be put in storage; the historical error data may be determined historically by the experimenter, the first error correction factor being, for example: +0.015. The historical error data comprises error quantity, the purpose of calculating the trigger index is to judge whether the data in the trigger frame is in a stable trend, namely whether the error condition is temperature or not, and if the data is stable, the error quantity can be used for calculating a first error correction coefficient; the trigger frame is a virtual frame of a time length. When the constructed error correction library is used, a current second matching scheme of the sensor is obtained, a corresponding second error correction coefficient is determined, and the measured value of the lead ion concentration is corrected correspondingly.
The foregoing description is only illustrative of the present invention and is not intended to limit the scope of the invention, and all equivalent structural changes made by the content of the present invention or direct or indirect application in other related technical fields are included in the scope of the present invention.
Claims (5)
1. A method for detecting lead ions by a sensor is characterized in that: the method comprises the following steps:
s1, preparing a sensor for detecting current intensity, wherein the sensor comprisesThe sensor is formed by mixing quantum dots, enzyme and enzyme substrates, wherein the adding volume ratio is 1:0.1:1, and the concentration of the quantum dots is 10 -6 ~10 -4 mol/L, wherein the concentration of the enzyme is 1-8U/mL, and the concentration of the enzyme substrate is 0.5-1 mol/L;
s2, placing the sensor in an electrolytic cell, and dividing the electrolytic cell into a reference area and a detection area by using an alumina membrane electrode, wherein the reference area is communicated with the detection area through the sensor; placing a working electrode in a reference area, placing a reference electrode in a detection area, and electrically connecting the working electrode, the reference electrode and an electrochemical workstation to assemble a detection system;
s3, electrolyte solution is added into the reference area and the detection area, detection potential is applied to the electrochemical workstation, then lead ion aqueous solution is added into the reference area, the change of photocurrent intensity between a reference electrode and a working electrode is measured according to the change of fluorescence intensity of quantum dots in the sensor, and the change of photocurrent intensity is analyzed by adopting a differential pulse voltammetry method to obtain a measured value of lead ion concentration, so that lead ion is detected;
s4, constructing an error correction library corresponding to the sensor, and correcting the measured value of the lead ion concentration based on the error correction library;
wherein constructing an error correction library corresponding to the sensor comprises:
obtaining a plurality of different first collocations of components mixed to form the sensor, the first collocations comprising: the volume ratio, the type and the concentration of each component;
acquiring a plurality of history error records corresponding to the first collocation scheme;
extracting an error amount in the history error record;
establishing a time axis, and representing the error amount on the time axis based on the record generation time of the history error record corresponding to the error amount;
acquiring a preset trigger frame, translating the trigger frame on the time axis, and calculating a two-to-two subtracted difference value of the error amount falling in the trigger frame each time in the translation process;
based on the error, a trigger index is calculated as follows:
;
;
wherein ,for the trigger index, +.>A two-by-two subtraction of the error amount falling in the trigger frame>Difference(s)>For a preset difference threshold, +.>For the total number of said differences +.>Is an intermediate variable;
if the trigger index is greater than or equal to a preset trigger index threshold, calculating an average value of the error amounts falling in the trigger frame;
after the trigger frame translates on the time axis, calculating a first error correction coefficient based on each average value, wherein the calculation formula is as follows:
;
wherein ,for said first error correction factor, +.>Is->Average value>A total number of the averages;
pairing the first error correction coefficient with the corresponding first collocation scheme to obtain a pairing item;
constructing an error correction library corresponding to the sensor based on each pairing item;
wherein correcting the measured value of the lead ion concentration based on the error correction library includes:
acquiring a current second collocation scheme of the sensor, and determining a second error correction coefficient corresponding to the second collocation scheme based on the error correction library;
and correcting the measured value of the lead ion concentration based on the second error correction coefficient, wherein a correction formula is as follows:
;
wherein ,for the corrected measurement of the lead ion concentration, +.>For the measurement of the lead ion concentration before correction, +.>For the second error correction coefficient;
the quantum dot is one of CdSe, cdS or PbS;
the enzyme is glutathione oxidase;
the enzyme substrate is glutathione.
2. A method for detecting lead ions by a sensor according to claim 1, wherein: the detection limit of the lead ions is 0.035nM.
3. A method for detecting lead ions by a sensor according to claim 1, wherein: the electrolyte solution is 1mmol/L NaCl solution.
4. A method for detecting lead ions by a sensor according to claim 1, wherein: the working electrode is an Ag/AgCl electrode.
5. A method for detecting lead ions by a sensor according to claim 1, wherein: the reference electrode is a platinum electrode.
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