CN109856218B - Modification material for preparing working electrode of biosensor - Google Patents
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Abstract
The invention relates to the technical field of novel functional materials, and discloses a modified material for preparing a working electrode of a biosensor.
Description
Technical Field
The invention belongs to the technical field of novel functional materials, and particularly relates to a modified material for preparing a working electrode of a biosensor.
Background
Sensors, also called inductors. Is a device that converts a physical or chemical quantity into an electrical signal for easy use. The definition of the national standard GB7665-87 for sensors is: "a device or apparatus which can sense a predetermined measured quantity and convert it into a usable signal according to a certain rule, generally consists of a sensing element and a converting element". The sensor is a detection device which can sense the information to be measured and convert the sensed information into an electric signal or other information in a required form according to a certain rule for output so as to meet the requirements of information transmission, processing, storage, display, recording, control and the like. The method is the first link for realizing automatic detection and automatic control. The definition of the international electrotechnical commission is: "Sensors are a type of pre-positioned component in a measurement system that converts input variables into signals that can be measured". According to the Gopel et al, are: "sensor is a sensitive element comprising a carrier and circuit connections" and "sensor system is a system incorporating some information processing (analog or digital) capability". The sensor is a component of the sensing system and is the first gateway into which the measured signal is input.
A biosensor is an instrument that is sensitive to a biological substance and converts its concentration into an electrical signal for detection. Is an analysis tool or system composed of immobilized biological sensitive material as recognition element (including enzyme, antibody, antigen, microbe, cell, tissue, nucleic acid, etc.), proper physicochemical transducer (such as oxygen electrode, photosensitive tube, field effect tube, piezoelectric crystal, etc.) and signal amplification device. The biosensor has the functions of a receptor and a transducer. With the development of biotechnology, the revolution of sensors is continuously ongoing, and particularly, the research on electrode materials is becoming more and more high-tech. Among the numerous electrode modification materials, noble metal materials are most used, but because they are expensive and easily adsorb impurities on the electrode surface, the detection accuracy and sensitivity are limited. The current need seeks a working electrode modification material with low cost, accurate detection and wide detection range.
Disclosure of Invention
The invention aims to solve the existing problems and provides a modified material for preparing a working electrode of a biosensor, which is further applied to the biosensor due to high sensitivity and low detection concentration and has the advantages of high detection sensitivity, low cost, wide detection range, long service life and the like.
The invention is realized by the following technical scheme:
a modification material for preparing a working electrode of a biosensor is prepared from the following components in parts by weight: 4.8-5.0 parts of magnesium acetate, 3.4-3.6 parts of tin oxide, 34-38 parts of ethanol, 40-45 parts of sodium citrate aqueous solution, 2.4-2.5 parts of o-phenylenediamine, 12-14 parts of polyvinyl alcohol, 3.5-4.0 parts of terpineol and 0.3-0.4 part of carboxymethyl cellulose; the preparation method comprises the following steps:
(1) adding a sodium citrate aqueous solution into a beaker, adding magnesium acetate at the rotating speed of 300-320 r/min, stirring and mixing for 35-40 min, sequentially adding tin oxide and o-phenylenediamine into an ethanol solution, uniformly stirring, heating to 70-75 ℃, performing reflux reaction for 2.5-3.0 h to obtain a reaction solution, neutralizing the reaction solution by using a saturated sodium carbonate solution at 25 ℃, adjusting the pH value to 7.4-7.6, then adding the reaction solution into a magnesium acetate mixed solution, and stirring and mixing for 20-30 min to obtain a uniform dispersion;
(2) transferring the uniform dispersion obtained in the step (1) into a high-pressure reaction kettle, setting the reaction temperature to be 180-190 ℃, reacting for 13-16 hours, cooling to room temperature after the reaction is finished, removing supernatant liquid, performing centrifugal separation on the obtained precipitate, sequentially washing for 3-5 times by using deionized water and absolute ethyl alcohol respectively, and then drying in an oven at 60-65 ℃ for 6-8 hours to obtain the multi-metal nano functional material;
(3) and (3) mixing the multi-metal nano functional material prepared in the step (2) with polyvinyl alcohol, terpineol and carboxymethyl cellulose according to the weight parts, continuously stirring for 50-60 minutes at the speed of 360 revolutions per minute of 340-.
As a further description of the above scheme, the pressure in the high-pressure reaction kettle in the step (2) is in the range of 0.45-0.50 MPa.
As a further description of the above scheme, the particle size of the multi-metal nano functional material is between 6 and 8 nanometers.
As a further description of the above scheme, the mass concentration of the sodium citrate aqueous solution is 5.5-6.0%.
As a further description of the above scheme, the specific surface area of the multi-metal nano functional material is between 330 and 335 square meters/gram.
Compared with the prior art, the invention has the following advantages: in order to solve the problem of poor performance of the modification material of the working electrode of the existing biosensor, the invention provides the modification material for preparing the working electrode of the biosensor, the prepared multi-metal nano functional material is mixed with polyvinyl alcohol, terpineol and carboxymethyl cellulose according to the weight parts, so that nano particles are uniformly distributed on a decorative slurry carrier, and the prepared working electrode has excellent detection performance, and the high sensitivity and the low detection concentration enable the working electrode to be further applied to the biosensor, and has the advantages of high detection sensitivity, low cost, wide detection range, long service life and the like, and has the performances of pollution prevention, interference resistance and the like The biosensor has the advantages of high specificity and high sensitivity, improves the function effect and the service life of the working electrode of the biosensor, reduces the cost, improves the development and the utilization of electrode modification materials, can realize the practical significance of promoting the development of the sensor industry and improving the application value in the fields of biomedicine and the like, and is a technical scheme which is extremely worthy of popularization and application.
Detailed Description
In order to make the objects, technical solutions and effects of the present invention clearer and clearer, the present invention is further described with reference to specific embodiments, and it should be understood that the specific embodiments described herein are only used for explaining the present invention and are not used for limiting the technical solutions provided by the present invention.
Example 1
A modification material for preparing a working electrode of a biosensor is prepared from the following components in parts by weight: 4.8 parts of magnesium acetate, 3.4 parts of tin oxide, 34 parts of ethanol, 40 parts of sodium citrate aqueous solution, 2.4 parts of o-phenylenediamine, 12 parts of polyvinyl alcohol, 3.5 parts of terpineol and 0.3 part of carboxymethyl cellulose; the preparation method comprises the following steps:
(1) adding a sodium citrate aqueous solution into a beaker, adding magnesium acetate at the rotating speed of 300 revolutions per minute, stirring and mixing for 35 minutes, sequentially adding tin oxide and o-phenylenediamine into an ethanol solution, uniformly stirring, heating to 70 ℃, carrying out reflux reaction for 2.5 hours to obtain a reaction solution, neutralizing the reaction solution by using a saturated sodium carbonate solution at the temperature of 25 ℃, adjusting the pH value to be 7.4-7.6, then adding the reaction solution into a magnesium acetate mixed solution, and stirring and mixing for 20-30 minutes to obtain a uniform dispersion;
(2) transferring the uniform dispersion obtained in the step (1) into a high-pressure reaction kettle, setting the reaction temperature to be 180 ℃, reacting for 13 hours, cooling to room temperature after the reaction is finished, removing supernatant liquid, performing centrifugal separation on the obtained precipitate, washing for 3 times by using deionized water and absolute ethyl alcohol respectively in sequence, and then drying in an oven at 60 ℃ for 6 hours to obtain the multi-metal nano functional material;
(3) and (3) mixing the multi-metal nano functional material prepared in the step (2) with polyvinyl alcohol, terpineol and carboxymethyl cellulose according to the weight parts, continuously stirring for 50 minutes at 340 revolutions per minute, and continuing ultrasonic treatment for 15 minutes to obtain viscous slurry, namely the modification material of the working electrode of the biosensor.
As a further description of the above scheme, the pressure in the high-pressure reaction kettle in the step (2) is in the range of 0.45-0.50 MPa.
As a further description of the above scheme, the particle size of the multi-metal nano functional material is between 6 and 8 nanometers.
As a further description of the above scheme, the mass concentration of the sodium citrate aqueous solution is 5.5%.
As a further description of the above scheme, the specific surface area of the multi-metal nano functional material is between 330 and 335 square meters/gram.
Example 2
A modification material for preparing a working electrode of a biosensor is prepared from the following components in parts by weight: 4.9 parts of magnesium acetate, 3.5 parts of tin oxide, 36 parts of ethanol, 42 parts of sodium citrate aqueous solution, 2.45 parts of o-phenylenediamine, 13 parts of polyvinyl alcohol, 3.8 parts of terpineol and 0.35 part of carboxymethyl cellulose; the preparation method comprises the following steps:
(1) adding a sodium citrate aqueous solution into a beaker, adding magnesium acetate at the rotating speed of 310 r/min, stirring and mixing for 38 min, sequentially adding tin oxide and o-phenylenediamine into an ethanol solution, uniformly stirring, heating to 72 ℃, carrying out reflux reaction for 2.8 h to obtain a reaction solution, neutralizing the reaction solution by using a saturated sodium carbonate solution at the temperature of 25 ℃, adjusting the pH value to be between 7.4 and 7.6, then adding the reaction solution into a magnesium acetate mixed solution, and stirring and mixing for 25 min to obtain a uniform dispersion;
(2) transferring the uniform dispersion obtained in the step (1) into a high-pressure reaction kettle, setting the reaction temperature to 185 ℃, reacting for 14 hours, cooling to room temperature after the reaction is finished, removing supernatant liquid, performing centrifugal separation on the obtained precipitate, washing for 4 times by using deionized water and absolute ethyl alcohol respectively in sequence, and then drying in an oven at 62 ℃ for 7 hours to obtain the multi-metal nano functional material;
(3) and (3) mixing the multi-metal nano functional material prepared in the step (2) with polyvinyl alcohol, terpineol and carboxymethyl cellulose according to the weight parts, continuously stirring for 55 minutes at the speed of 350 revolutions per minute, and continuously carrying out ultrasonic treatment for 18 minutes to obtain viscous slurry, namely the modification material of the working electrode of the biosensor.
As a further description of the above scheme, the pressure in the high-pressure reaction kettle in the step (2) is in the range of 0.45-0.50 MPa.
As a further description of the above scheme, the particle size of the multi-metal nano functional material is between 6 and 8 nanometers.
As a further description of the above scheme, the mass concentration of the sodium citrate aqueous solution is 5.8%.
As a further description of the above scheme, the specific surface area of the multi-metal nano functional material is between 330 and 335 square meters/gram.
Example 3
A modification material for preparing a working electrode of a biosensor is prepared from the following components in parts by weight: 5.0 parts of magnesium acetate, 3.6 parts of tin oxide, 38 parts of ethanol, 45 parts of sodium citrate aqueous solution, 2.5 parts of o-phenylenediamine, 14 parts of polyvinyl alcohol, 4.0 parts of terpineol and 0.4 part of carboxymethyl cellulose; the preparation method comprises the following steps:
(1) adding a sodium citrate aqueous solution into a beaker, adding magnesium acetate at the rotating speed of 320 revolutions per minute, stirring and mixing for 40 minutes, sequentially adding tin oxide and o-phenylenediamine into an ethanol solution, uniformly stirring, heating to 75 ℃, carrying out reflux reaction for 3.0 hours to obtain a reaction solution, neutralizing the reaction solution by using a saturated sodium carbonate solution at the temperature of 25 ℃, adjusting the pH value to be between 7.4 and 7.6, then adding the reaction solution into a magnesium acetate mixed solution, and stirring and mixing for 30 minutes to obtain a uniform dispersion;
(2) transferring the uniform dispersion obtained in the step (1) into a high-pressure reaction kettle, setting the reaction temperature to be 190 ℃, reacting for 16 hours, cooling to room temperature after the reaction is finished, removing supernatant liquid, performing centrifugal separation on the obtained precipitate, washing for 5 times by using deionized water and absolute ethyl alcohol respectively in sequence, and then drying in an oven at 65 ℃ for 8 hours to obtain the multi-metal nano functional material;
(3) and (3) mixing the multi-metal nano functional material prepared in the step (2) with polyvinyl alcohol, terpineol and carboxymethyl cellulose according to the weight parts, continuously stirring for 60 minutes at 360 revolutions per minute, and continuing ultrasonic treatment for 20 minutes to obtain viscous slurry, namely the modification material of the working electrode of the biosensor.
As a further description of the above scheme, the pressure in the high-pressure reaction kettle in the step (2) is in the range of 0.45-0.50 MPa.
As a further description of the above scheme, the particle size of the multi-metal nano functional material is between 6 and 8 nanometers.
As a further description of the above scheme, the mass concentration of the sodium citrate aqueous solution is 6.0%.
As a further description of the above scheme, the specific surface area of the multi-metal nano functional material is between 330 and 335 square meters/gram.
Comparative example 1
The difference from example 1 is only that the addition of magnesium acetate is omitted in the preparation of the modified material of the working electrode of the biosensor, and the rest is kept consistent.
Comparative example 2
The difference from example 2 is only that in the preparation of the modified material of the biosensor working electrode, the addition of the tin oxide is omitted, and the rest is kept consistent.
Comparative example 3
The difference from example 3 is only that deionized water is used instead of the sodium citrate aqueous solution in the preparation of the modified material of the biosensor working electrode, and the rest is kept consistent.
Comparative example 4
The difference from example 3 is only that in the preparation of the modified material of the biosensor working electrode, the addition of o-phenylenediamine is omitted, and the rest is kept consistent.
Comparative example 5
The only difference from example 3 is that in the preparation of the modified material of the working electrode of the biosensor, the temperature was raised to 200 ℃ and the reaction was carried out for 12 hours, and the rest was kept the same.
Comparative experiment
Using the modified materials of the working electrodes of the biosensors in the methods of examples 1 to 3 and comparative examples 1 to 5, respectively, the electrochemical biosensors respectively constructed by using the method of depositing nanogold as the modified material by an electrodeposition method as a control group, using a glassy carbon electrode as the working electrode and based on the same sensor parts, and using the same electroanalytical means, processing the manufactured sensors according to the methods of each group for detecting glucose, wherein the glucose concentration range is 0.15uM-2mM, performing performance tests on the samples of each group under the same test conditions, collecting representative data when the data is stable, obtaining the average value of 5 groups of samples, keeping the independent variables in the test consistent, and counting the effective average value, wherein the results are shown in the following table:
the modification material for preparing the working electrode of the biosensor solves the problem of poor performance of the modification material of the working electrode of the existing biosensor, has the advantages of rapid and rapid detection, high specificity and high sensitivity, improves the function effect and the service life of the working electrode of the biosensor, reduces the cost, improves the development and the utilization of the electrode modification material, can realize the practical significance of promoting the development of the sensor industry and improving the application value in the fields of biomedicine and the like, and is a technical scheme which is extremely worthy of popularization and use.
Claims (5)
1. A modification material for preparing a working electrode of a biosensor is characterized by being prepared from the following components in parts by weight: 4.8-5.0 parts of magnesium acetate, 3.4-3.6 parts of tin oxide, 34-38 parts of ethanol, 40-45 parts of sodium citrate aqueous solution, 2.4-2.5 parts of o-phenylenediamine, 12-14 parts of polyvinyl alcohol, 3.5-4.0 parts of terpineol and 0.3-0.4 part of carboxymethyl cellulose; the preparation method comprises the following steps:
(1) adding a sodium citrate aqueous solution into a beaker, adding magnesium acetate at the rotating speed of 300-320 r/min, stirring and mixing for 35-40 min, sequentially adding tin oxide and o-phenylenediamine into an ethanol solution, uniformly stirring, heating to 70-75 ℃, performing reflux reaction for 2.5-3.0 h to obtain a reaction solution, neutralizing the reaction solution by using a saturated sodium carbonate solution at 25 ℃, adjusting the pH value to 7.4-7.6, then adding the reaction solution into a magnesium acetate mixed solution, and stirring and mixing for 20-30 min to obtain a uniform dispersion;
(2) transferring the uniform dispersion obtained in the step (1) into a high-pressure reaction kettle, setting the reaction temperature to be 180-190 ℃, reacting for 13-16 hours, cooling to room temperature after the reaction is finished, removing supernatant liquid, performing centrifugal separation on the obtained precipitate, sequentially washing for 3-5 times by using deionized water and absolute ethyl alcohol respectively, and then drying in an oven at 60-65 ℃ for 6-8 hours to obtain the multi-metal nano functional material;
(3) and (3) mixing the multi-metal nano functional material prepared in the step (2) with polyvinyl alcohol, terpineol and carboxymethyl cellulose according to the weight parts, continuously stirring for 50-60 minutes at the speed of 360 revolutions per minute of 340-.
2. The modified material for preparing a working electrode of a biosensor as claimed in claim 1, wherein the pressure in the autoclave in step (2) is in the range of 0.45-0.50 MPa.
3. The modified material for preparing a working electrode of a biosensor as claimed in claim 1, wherein the particle size of the multi-metallic nano-functional material is between 6 and 8 nm.
4. The modified material for preparing a working electrode of a biosensor as claimed in claim 1, wherein the mass concentration of the sodium citrate aqueous solution is 5.5-6.0%.
5. The modified material of claim 1, wherein the specific surface area of the multi-metal nano-functional material is between 330 and 335 m/g.
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