CN109254069B - Modified electrode and electrochemical detection method of sulpiride - Google Patents
Modified electrode and electrochemical detection method of sulpiride Download PDFInfo
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- CN109254069B CN109254069B CN201810884649.2A CN201810884649A CN109254069B CN 109254069 B CN109254069 B CN 109254069B CN 201810884649 A CN201810884649 A CN 201810884649A CN 109254069 B CN109254069 B CN 109254069B
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- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
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- G—PHYSICS
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Abstract
The invention discloses an electrochemical detection method of sulpiride, which comprises the following steps: method for preparing alpha-MoO by hydrothermal synthesis3Powder, and the alpha-MoO is prepared by adopting a thermal evaporation method3Depositing on the surface of the pretreated glassy carbon electrode in the form of a nanorod; preparing sulpiride into standard solutions with different concentrations by adopting Tris-HCl, adjusting the pH value of the solution, and mixing alpha-MoO3Soaking the nanorod modified glassy carbon electrode in a solution to perform differential pulse voltammetry detection, making a standard curve of peak current-concentration, and displaying a good linear relation; and (3) placing the modified electrode in a solution to be detected for detection, and calculating according to a standard curve to obtain the concentration of the sulpiride in the solution to be detected. The method can rapidly measure the concentration of sulpiride, and the detection limit is 1.0 multiplied by 10‑8mol/L, linear range 5.0X 10‑8～1.0×10‑5And the sensitivity is high.
Description
Technical Field
The invention relates to a modified electrode and application thereof, and further relates to alpha-MoO3A nanorod modified glassy carbon electrode and application thereof in electrochemical detection of sulpiride are disclosed.
Background
Sulpiride, also known as antiemetic, is a sulfonamide derivative, is a selective antagonist of central dopamine receptors, has strong antipsychotic and antiemetic effects, also has a psychotropic effect, has good curative effects on symptoms such as apathy, retraction, mumps, depression, hallucinations, delusions and the like, and is a psychotropic drug which develops rapidly in recent years.
The methods for measuring the sulpiride content and pharmacokinetics mainly comprise an ultraviolet absorption spectrometry, a fluorescence photometry, a thin layer scanning method, a capillary electrophoresis method and the like, and the chromatographic or spectroscopic analysis methods have the defects of expensive equipment, complex operation, long analysis time and the like, so that improvement is urgently needed.
Molybdenum oxide has the advantages of wider band gap, smaller resistivity, higher catalytic activity and the like, and attracts attention in recent years, molybdenum oxide is commonly used as a modifying material of a gas sensor, but a molybdenum oxide nanorod modified glassy carbon electrode and a method for electrochemical detection of sulpiride by using the same are not reported so far. The invention provides an electrochemical modified electrode and a detection method for solving the problems of low efficiency of sulpiride detection by chromatography or spectrometry and improving the electrochemical catalytic effect and detection sensitivity of electrochemical detection of sulpiride.
Disclosure of Invention
The invention aims to provide a preparation method of a molybdenum oxide nanorod modified electrode, which is used for electrochemical detection of sulpiride, so that the catalytic effect of electrochemical detection of sulpiride is improved, and the detection efficiency and sensitivity are improved.
The purpose of the invention is realized as follows: alpha-MoO3The preparation method of the nanorod modified glassy carbon electrode is characterized by comprising the following steps:
(1)α-MoO3preparation of powder: anhydrous sodium molybdate and hydrochloric acid are mixed according to a molar ratio of 1: 3-7, transferring the dispersion liquid into a polytetrafluoroethylene high-pressure reaction kettle, placing the reaction kettle in a heating device, carrying out hydrothermal reaction for 1-4 h at 150-190 ℃, naturally cooling to room temperature, filtering, drying, placing in a tubular furnace, calcining for 1-4 h at 350-500 ℃ in an air atmosphere to obtain alpha-MoO3Powder;
(2) pretreating a glassy carbon electrode: polishing the glassy carbon electrode with 0.1 micron and 0.05 micron of alumina powder for 2min in sequence, polishing to a mirror surface, and ultrasonically cleaning the polished glassy carbon electrode with acetone and deionized water for 3min respectively to obtain a pretreated glassy carbon electrode;
(3)α-MoO3and (3) modifying the glassy carbon electrode by the nano rod: by using the prepared alpha-MoO3The material is prepared by evaporating alpha-MoO under vacuum condition3Depositing on the surface of the pretreated glassy carbon electrode to form alpha-MoO3And (3) modifying the glassy carbon electrode by the nanorod.
Further, the molar ratio of the anhydrous sodium molybdate to the hydrochloric acid is 1: 5, the temperature of the hydrothermal reaction is 170 ℃, the calcining temperature is 400 ℃, and the calcining time is 2 h.
Further, the vacuum deposition conditions were: pressure 2X 10-5mbar, temperature 250 ℃.
Further, the application is to convert alpha-MoO3Nanorod modificationThe glassy carbon electrode is used for electrochemical detection of sulpiride.
Further, the detection method comprises the following steps:
a. to prepare the resulting alpha-MoO3The nanorod modified glassy carbon electrode is used as a working electrode, the platinum wire is used as a counter electrode, and the saturated calomel electrode is used as a reference electrode to form a three-electrode system;
b. preparing standard solutions with different concentrations from sulpiride by adopting Tris-HCl, adjusting the pH value of the solution to 5-7, immersing a three-electrode system in the solution to carry out differential pulse voltammetry detection, wherein the scanning voltage is-1.5V-0V, and the scanning rate is 50-100 mV/s; making a peak current-concentration standard curve, displaying a good linear relation, and performing linear fitting to obtain a linear equation of the standard solution; and (3) placing the modified electrode in a solution to be detected for detection, and calculating according to the peak current value and a linear equation to obtain the concentration of the sulpiride in the solution to be detected.
Further, the pH value of the solution is adjusted to be 6 before detection, and the parameters of the differential pulse voltammetry are as follows: the scanning voltage is-1.5V-0V, the scanning speed is 100mV/s, the potential increment is 5mV, the pulse width is 50mV, the pulse period is 0.5s, the sampling width is 0.02s, and the standing time is 2 s; detection limit of 1.0 x 10-8mol/L, linear range 5.0X 10-8～1.0×10-5mol/L。
Compared with the prior art, the invention has the following beneficial effects:
(1) the invention firstly prepares alpha-MoO3Powder and then preparing alpha-MoO by adopting a vacuum evaporation method3The nanorod modified glassy carbon electrode is simple in preparation method and high in electrochemical activity.
(2) The invention discovers alpha-MoO3High electrochemical catalytic activity of nano-rod on sulpiride and use of alpha-MoO3The nano-rod modified glassy carbon electrode realizes electrochemical detection of sulpiride by differential pulse voltammetry.
(3) Compared with a chromatographic or spectral detection method, the method has the advantages of high detection sensitivity, wide linear range, low detection limit, simplicity and high application value.
Drawings
FIG. 1 is a view of alpha-MoO3The nano-rod modified electrode is in a sulpiride solution prepared from Tris-HCl with the pH value of 6, and a linear correlation curve of peak current and sulpiride concentration is obtained by detecting sulpiride with different concentrations through a differential pulse voltammetry.
Detailed Description
The invention is further described with reference to the accompanying drawings, which are not intended to be limiting in any way, and any variations based on the teachings of the invention are intended to fall within the scope of the invention.
Example 1
Preparation of alpha-MoO3And (3) modifying the glassy carbon electrode by the nano rod:
(1)α-MoO3preparation of powder: anhydrous sodium molybdate and hydrochloric acid are mixed according to a molar ratio of 1: 3 in proportion, transferring the dispersion liquid into a polytetrafluoroethylene high-pressure reaction kettle, placing the reaction kettle in a heating device, carrying out hydrothermal reaction for 1h at 150 ℃, naturally cooling to room temperature, filtering, drying, then placing in a tubular furnace, calcining for 1h at 350 ℃ in air atmosphere to obtain alpha-MoO3Powder;
(2) pretreating a glassy carbon electrode: polishing the glassy carbon electrode with 0.1 micron and 0.05 micron of alumina powder for 2min in sequence, polishing to a mirror surface, and ultrasonically cleaning the polished glassy carbon electrode with acetone and deionized water for 3min respectively to obtain a pretreated glassy carbon electrode;
(3)α-MoO3and (3) modifying the glassy carbon electrode by the nano rod: by using the prepared alpha-MoO3The material is prepared by evaporating alpha-MoO under vacuum condition3Depositing on the surface of the pretreated glassy carbon electrode to form alpha-MoO3And (3) modifying the glassy carbon electrode by the nanorod.
Example 2
Preparation of alpha-MoO3And (3) modifying the glassy carbon electrode by the nano rod:
(1)α-MoO3preparation of powder: anhydrous sodium molybdate and hydrochloric acid are mixed according to a molar ratio of 1: 7 in deionized water, transferring the dispersion into a polytetrafluoroethylene high-pressure reaction kettle, placing the reaction kettle in a heating device, carrying out hydrothermal reaction at 190 ℃ for 4 hours, naturally cooling to room temperature, filtering, and dryingThen placing the mixture into a tubular furnace, calcining the mixture for 4 hours at 500 ℃ in air atmosphere to obtain alpha-MoO3Powder;
(2) pretreating a glassy carbon electrode: polishing the glassy carbon electrode with 0.1 micron and 0.05 micron of alumina powder for 2min in sequence, polishing to a mirror surface, and ultrasonically cleaning the polished glassy carbon electrode with acetone and deionized water for 3min respectively to obtain a pretreated glassy carbon electrode;
(3)α-MoO3and (3) modifying the glassy carbon electrode by the nano rod: by using the prepared alpha-MoO3The material is prepared by evaporating alpha-MoO under vacuum condition3Depositing on the surface of the pretreated glassy carbon electrode to form alpha-MoO3And (3) modifying the glassy carbon electrode by the nanorod.
Example 3
α-MoO3Preparing a nanorod modified glassy carbon electrode:
(1)α-MoO3preparation of powder: anhydrous sodium molybdate and hydrochloric acid are mixed according to a molar ratio of 1: 5 in deionized water, transferring the dispersion into a polytetrafluoroethylene high-pressure reaction kettle, placing the reaction kettle in a heating device, carrying out hydrothermal reaction for 2 hours at 170 ℃, naturally cooling to room temperature, filtering, drying, placing in a tubular furnace, calcining for 2 hours at 400 ℃ in air atmosphere to obtain alpha-MoO3Powder;
(2) pretreating a glassy carbon electrode: polishing the glassy carbon electrode with 0.1 micron and 0.05 micron of alumina powder for 2min in sequence, polishing to a mirror surface, and ultrasonically cleaning the polished glassy carbon electrode with acetone and deionized water for 3min respectively to obtain a pretreated glassy carbon electrode;
(3)α-MoO3and (3) modifying the glassy carbon electrode by the nano rod: by using the prepared alpha-MoO3The material is prepared by evaporating alpha-MoO under vacuum condition3Depositing on the surface of the pretreated glassy carbon electrode to form alpha-MoO3And (3) modifying the glassy carbon electrode by the nanorod.
TEM analysis shows that the surface of the electrode is successfully modified by alpha-MoO3Material, alpha-MoO3Is attached to the surface of the electrode in a nanorod form.
Example 4
α-MoO3Detection of sulpiride by nanorod modified glassy carbon electrode
a. EXAMPLE 3 alpha-MoO prepared3The nanorod modified glassy carbon electrode is used as a working electrode, the platinum wire is used as a counter electrode, and the saturated calomel electrode is used as a reference electrode to form a three-electrode system;
b. preparing standard solutions with different concentrations by using Tris-HCl, adjusting the pH value of the solutions to be 6, sequentially immersing a three-electrode system in each solution (in the order of the concentration from small to large) to carry out differential pulse voltammetry, wherein the scanning voltage is-1.5V-0V, the scanning rate is 100mV/s, the potential increment is 5mV, the pulse width is 50mV, the pulse period is 0.5s, the sampling width is 0.02s, and the standing time is 2 s; differential pulse voltammetry showed that a peak current developed at-1.2V, which increased with increasing sulpiride concentration. And (3) making a peak current-concentration standard curve, displaying a good linear relation, and performing linear fitting to obtain a linear equation of the standard solution.
FIG. 1 is a view of alpha-MoO3The nano-rod modified electrode is in a sulpiride solution prepared from Tris-HCl with the pH value of 6, and a linear correlation curve of peak current and sulpiride concentration is obtained by detecting sulpiride with different concentrations through a differential pulse voltammetry. The linear regression equation is calculated as follows: i-95.96 c + 6.5; wherein, I is peak current with the unit of muA, and c is the concentration of the sulpiride solution with the unit of mumol/L.
Linear range 5.0 x 10-8～1.0×10-5mol/L, detection limit 1.0X 10-8mol/L。
And (3) placing the three-electrode system in a sulpiride solution to be detected with unknown concentration for detection, and calculating the concentration of sulpiride in the solution to be detected according to the peak current value and a linear equation.
The foregoing is directed to the preferred embodiment of the present invention and is not intended to limit the invention to the specific embodiment described. It will be apparent to those skilled in the art that various modifications, equivalents, improvements and the like can be made without departing from the spirit of the invention, and these are intended to be included within the scope of the invention.
Claims (5)
1. alpha-MoO3The application of the nanorod modified glassy carbon electrode is characterized in that alpha-MoO is used3The nanorod modified glassy carbon electrode is used for electrochemically detecting sulpiride, and the alpha-MoO3The preparation method of the nanorod modified glassy carbon electrode comprises the following steps:
(1)α-MoO3preparation of powder: anhydrous sodium molybdate and hydrochloric acid are mixed according to a molar ratio of 1: 3-7, transferring the dispersion liquid into a polytetrafluoroethylene high-pressure reaction kettle, placing the reaction kettle in a heating device, carrying out hydrothermal reaction for 1-4 h at 150-190 ℃, naturally cooling to room temperature, filtering, drying, placing in a tubular furnace, calcining for 1-4 h at 350-500 ℃ in an air atmosphere to obtain alpha-MoO3Powder;
(2) pretreating a glassy carbon electrode: polishing the glassy carbon electrode with 0.1 micron and 0.05 micron of alumina powder for 2min in sequence, polishing to a mirror surface, and ultrasonically cleaning the polished glassy carbon electrode with acetone and deionized water for 3min respectively to obtain a pretreated glassy carbon electrode;
(3)α-MoO3and (3) modifying the glassy carbon electrode by the nano rod: by using the prepared alpha-MoO3The material is prepared by evaporating alpha-MoO under vacuum condition3Depositing on the surface of the pretreated glassy carbon electrode to form alpha-MoO3And (3) modifying the glassy carbon electrode by the nanorod.
2. alpha-MoO according to claim 13The application of the nanorod modified glassy carbon electrode is characterized in that the molar ratio of anhydrous sodium molybdate to hydrochloric acid is 1: 5, the temperature of the hydrothermal reaction is 170 ℃, the time of the hydrothermal reaction is 2 hours, the calcining temperature is 400 ℃, and the calcining time is 2 hours.
3. alpha-MoO according to claim 13The application of the nanorod modified glassy carbon electrode is characterized in that the vacuum evaporation conditions are as follows: pressure 2X 10-5mbar, temperature 250 ℃.
4. The use according to claim 1, wherein the method of detecting comprises the steps of:
a. alpha-MoO prepared by the process of claim 13The nanorod modified glassy carbon electrode is used as a working electrode, the platinum wire is used as a counter electrode, and the saturated calomel electrode is used as a reference electrode to form a three-electrode system;
b. preparing standard solutions with different concentrations and pH values of 5-7 by using Tris-HCl, immersing a three-electrode system in the solution to perform differential pulse voltammetry, wherein the scanning voltage is-1.5V-0V, and the scanning speed is 50-100 mV/s; making a peak current-concentration standard curve, displaying a good linear relation, and performing linear fitting to obtain a linear equation of the standard solution; and (3) placing the modified electrode in a solution to be detected for detection, and calculating according to the peak current value and a linear equation to obtain the concentration of the sulpiride in the solution to be detected.
5. The use of claim 4, wherein the pH of the conditioning solution prior to detection is 6 and the differential pulse voltammetry parameters are: the scanning voltage is-1.5V-0V, the potential increment is 5mV, the pulse width is 50mV, the pulse period is 0.5s, the sampling width is 0.02s, and the standing time is 2 s; detection limit of 1.0 x 10-8mol/L, linear range 5.0X 10-8～1.0×10-5mol/L。
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