CN114280123B - Preparation method of photoelectrochemical sensor for tetracycline detection - Google Patents
Preparation method of photoelectrochemical sensor for tetracycline detection Download PDFInfo
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Abstract
The invention relates to a preparation method of a photoelectrochemical sensor for tetracycline detection. The invention uses the indium sulfide nano material sensitized AgBiS 2 Obtaining an anodic photocurrent as a substrate material, agBiS 2 Is a nano material with excellent photoelectric activity, and the photocurrent response is greatly increased after indium sulfide sensitization. The tetracycline to be detected is directly dissolved in the electrolyte solution, so that the sensitivity of detection is effectively improved, and the sensitive detection of the tetracycline is realized. The detection limit is 0.022nmol/L.
Description
Technical Field
The invention relates to a preparation method of a photoelectrochemical sensor for tetracycline detection. Specifically, indium sulfide is adopted to sensitize AgBiS 2 The nano flower is used as a substrate photosensitive material to obtain anode photocurrent, and the tetracycline to be detected is directly dissolved in a test electrolyte solution to prepare a photoelectrochemical sensor for sensitively detecting the tetracycline, which belongs to the technical field of novel functional materials and sensing detection.
Background
Tetracycline hydrochloride is a broad-spectrum antibiotic, has inhibition effect on most gram-positive and gram-negative bacteria, has bactericidal effect at high concentration, can inhibit rickettsia, trachoma virus and the like, and has better effect on gram-negative bacteria. The action mechanism is mainly to prevent the combination of aminoacyl and ribonucleoprotein, prevent the growth of peptide chain and the synthesis of protein, thereby inhibiting the growth of bacteria and having bactericidal effect at high concentration. Tetracyclines are antibiotics that are widely used in veterinary and human therapy. Tetracyclines may be present in foods because they are overused in veterinary medicine as growth promoters and antibiotics. Residues of these antibiotics in food products can adversely affect human health and bacterial resistance to tetracycline antibiotics occurs in humans and veterinary medicine. Liver damage, anaphylaxis and yellowing of teeth are common side effects of tetracyclines. Therefore, sensitive and specific methods for detecting tetracyclines in serum and food products are necessary. Common methods for detecting glutathione include fluorescence analysis, colorimetric analysis, electrochemical analysis, and the like. However, the fluorescence analysis method is often complicated to operate and has a narrow detection linear range; the colorimetric analysis detection error is large; the electrochemical analysis time is long. The invention designs a novel photoelectrochemical sensor to realize the sensitive detection of the tetracycline, and has the advantages of high analysis speed, simple operation and good stability, and the detection limit of the photoelectrochemical sensor designed by the invention on the tetracycline reaches 0.022nmol/L.
AgBiS 2 The semiconductor nanomaterial has the advantages of good photocatalytic performance and photoelectric performance, simple preparation method, no toxicity, certain photostability and thermal stability, and photo-generated charges can be generated under the irradiation of visible light to form photocurrent, but the band gap width is narrow, and photo-generated electrons and holes can be rapidly compounded after being excited by the visible light, so that the utilization rate of the visible light is greatly reduced. Indium sulfide is used as an excellent sensitization material, and has the advantages of simple preparation, high yield and good stability. Nanometer flower-like AgBiS 2 The specific surface area of (2) is large, and a large amount of AgBiS2 can be loaded by sensitization of indium sulfide, so that excellent photoelectric performance is obtained. The tetracycline to be detected is directly dissolved in the photoelectrochemical test electrolyte solution, and is used as an electron donor in the test process, and the photocurrent signal obtained by the test is gradually increased along with the increase of the concentration of the tetracycline, so that the detection sensitivity of the sensor is improved, and the detection sensitivity of the sensor is greatly improved.
Photoelectrochemical sensors are a type of detection device that determines the concentration of an analyte based on the photoelectric conversion characteristics of the substance. The photoelectrochemistry detection method has the characteristics of simple equipment, high sensitivity and easy miniaturization, has been developed into an analysis method with great application potential, and has wide application prospect in the fields of food, environment, medicine and the like. Indium sulfide sensitized AgBiS 2 The application of the nano material in the photoelectrochemical sensor is not reported. The invention relates to an AgBiS based on indium sulfide sensitization 2 The nano material successfully constructs the photoelectrochemical sensor for detecting the tetracycline under the visible light. The sensor is sensitive to indium sulfideConverted nano flower-like AgBiS 2 As a substrate photosensitive material, the tetracycline to be detected is directly dissolved in a test electrolyte solution, so that the tetracycline is sensitively detected. The photoelectrochemical sensor prepared by the invention has the advantages of low cost, high sensitivity, good specificity, rapid detection, easy preparation and the like, realizes the rapid and high-sensitivity detection of glutathione in a visible light region, and effectively overcomes the defects of the existing tetracycline detection method.
Disclosure of Invention
One of the objects of the present invention is AgBiS sensitized with indium sulfide 2 The nanoflower material is used as a photosensitive material. The photosensitive material has excellent photoelectric performance and extremely high photoelectric conversion efficiency under visible light.
The second purpose of the invention is to directly dissolve the tetracycline to be detected in the test base solution, so that the sensitivity of detection is greatly improved.
The third object of the present invention is to use indium sulfide-AgBiS 2 The nano material is used as a substrate to prepare the photoelectrochemical sensor with high sensitivity, good stability and high detection speed, and the aim of sensitively detecting the tetracycline under the condition of visible light is fulfilled.
The technical scheme of the invention is as follows:
1. a preparation method of a photoelectrochemical sensor for tetracycline detection comprises the following steps:
（1）AgBiS 2 preparation of nanoflower
Dissolving 0.1-0.5 g silver nitrate, 0.3-0.7 g bismuth chloride and 0.2-0.6 g L-cysteine in 10-50 mL N, N-dimethylformamide, stirring at room temperature to 1-3 h, transferring the solution into a high-pressure reaction kettle, reacting at 150-220 ℃ for 10-16 h, centrifuging and washing the obtained product with absolute ethyl alcohol and ultrapure water after the reaction is finished, and vacuum drying at 35-65 ℃ to obtain AgBiS 2 A nanoflower;
(2) Preparation of indium sulfide nanomaterial
Dissolving 0.3-0.7 g sodium sulfate nonahydrate and 0.1-0.5 g indium nitrate hydrate into 30-80 mL ultrapure water, stirring uniformly at room temperature, transferring the solution into a high-pressure reaction kettle, reacting at 150-220 ℃ for 10-16 h, cooling to room temperature after the reaction is finished, washing the obtained black product with ultrapure water and absolute ethyl alcohol, and vacuum drying at 40-80 ℃ to obtain indium sulfide nanometer;
(3) Preparation of photoelectrochemical sensor
1) Ultrasonically cleaning conductive glass sequentially by using a surfactant, acetone, ethanol and ultrapure water, introducing nitrogen gas into a 70 ℃ oven for drying;
2) Taking AgBiS with concentration of 25 mu L of 5-10 mg/mL 2 Dripping the aqueous solution on the conductive surface of the ITO conductive glass, and baking under an infrared lamp;
3) Continuously dripping 20 mu L of indium sulfide aqueous solution with the concentration of 1-5 mg/mL on the surface of the modified electrode, and naturally airing the electrode at room temperature in a dark place; a photosensitive electrode for detecting tetracycline is prepared.
2. The detection method of the photosensitive electrode prepared by the preparation method is characterized by comprising the following steps:
(1) Using an electrochemical workstation to test by using a three-electrode system, wherein a saturated calomel electrode is used as a reference electrode, a platinum electrode is used as an auxiliary electrode, and the prepared ITO modified photosensitive electrode is used as a working electrode, and is tested in a PBS buffer solution with pH of 5.0-8.0 and containing 0.05-300 nmol/L glutathione;
(2) Detecting the tetracycline by a time-current method, setting the voltage to be-0.1V, the running time to be 120 s, and the wavelength of a light source to be 400-450 nm;
(3) After the electrodes are placed, the lamp is turned on every 10 s to continuously irradiate 10 s, record photocurrent, and draw a working curve;
(4) And (3) detecting the tetracycline sample solution to be detected instead of the tetracycline standard solution.
The detection linear range of the sensor for the tetracycline is 0.05-300 nmol/L, and the detection limit is 0.022nmol/L.
The chemicals required for the synthesis of the materials were purchased from local reagent shops and were not reprocessed.
Advantageous results of the invention
(1) The invention successfully synthesizes the preparation method with a singleFlower-like AgBiS with fixed photoelectric property 2 The nano material has low preparation cost, no toxicity and large specific surface area; agBiS with good sensitization by indium sulfide 2 Sensitization is carried out, excellent photoelectric property is obtained, and the problem of simple AgBiS is solved 2 And low photoelectric conversion efficiency of indium sulfide.
(2) According to the invention, the to-be-detected object is directly dissolved in the photoelectrochemical test electrolyte solution, and the photoelectric signal is gradually increased along with the increase of the concentration of the to-be-detected object, so that the sensitive detection of tetracycline is realized.
(4) The photoelectrochemical sensor prepared by the invention is used for detecting tetracycline peptide, has short response time, wide linear range, low detection limit, good stability and reproducibility, and can realize simple, rapid, high-sensitivity and specific detection. The detection linear range of the invention for the tetracycline is 0.05-300 nmol/L, and the detection limit reaches 0.022nmol/L.
Detailed description of the preferred embodiments
Example 1 preparation of photoelectrochemical sensor
（1）AgBiS 2 Preparation of nanoflower
Dissolving 0.1 g silver nitrate, 0.3 g bismuth chloride and 0.2 g L-cysteine in 10 mL N, N-dimethylformamide, stirring at room temperature for 1 h, transferring the solution into a high-pressure reaction kettle, reacting at 150deg.C for 10 h, centrifuging and washing the obtained product with absolute ethanol and ultrapure water, and vacuum drying at 35deg.C to obtain AgBiS 2 A nanoflower;
(2) Preparation of indium sulfide nanomaterial
Dissolving 0.3 g sodium sulfate nonahydrate and 0.1 g indium nitrate hydrate into 30 mL ultrapure water, stirring uniformly at room temperature, transferring the solution into a high-pressure reaction kettle, reacting at 150 ℃ for 10 h, cooling to room temperature after the reaction is finished, washing the obtained black product with the ultrapure water and absolute ethyl alcohol, and vacuum drying at 40 ℃ to obtain indium sulfide nanometer;
(3) Preparation of photoelectrochemical sensor
1) Ultrasonically cleaning conductive glass sequentially by using a surfactant, acetone, ethanol and ultrapure water, introducing nitrogen gas into a 70 ℃ oven for drying;
2) 25 mu L of AgBiS with concentration of 5 mg/mL is taken 2 Dripping the aqueous solution on the conductive surface of the ITO conductive glass, and baking under an infrared lamp;
3) Continuously dripping 20 mu L of indium sulfide aqueous solution with the concentration of 1 mg/mL on the surface of the modified electrode, and naturally airing at room temperature in a dark place; a photosensitive electrode for detecting tetracycline is prepared.
Example 2 preparation of photoelectrochemical sensor
（1）AgBiS 2 Preparation of nanoflower
Dissolving 0.1-0.5 g silver nitrate, 0.3-0.7 g bismuth chloride and 0.2-0.6 g L-cysteine in 10-50 mL N, N-dimethylformamide, stirring at room temperature to 1-3 h, transferring the solution into a high-pressure reaction kettle, reacting at 150-220 ℃ for 10-16 h, centrifuging and washing the obtained product with absolute ethyl alcohol and ultrapure water after the reaction is finished, and vacuum drying at 35-65 ℃ to obtain AgBiS 2 A nanoflower;
(2) Preparation of indium sulfide nanomaterial
Dissolving 0.5 g sodium sulfate nonahydrate and 0.3 g indium nitrate hydrate into 50 mL ultrapure water, stirring uniformly at room temperature, transferring the solution into a high-pressure reaction kettle, reacting at 160 ℃ for 12 h, cooling to room temperature after the reaction is finished, washing the obtained black product with the ultrapure water and absolute ethyl alcohol, and vacuum drying at 60 ℃ to obtain indium sulfide nanometer;
(3) Preparation of photoelectrochemical sensor
1) Ultrasonically cleaning conductive glass sequentially by using a surfactant, acetone, ethanol and ultrapure water, introducing nitrogen gas into a 70 ℃ oven for drying;
2) 25 mu L of AgBiS with concentration of 6 mg/mL is taken 2 Dripping the aqueous solution on the conductive surface of the ITO conductive glass, and baking under an infrared lamp;
3) Continuously dripping 20 mu L of indium sulfide aqueous solution with the concentration of 2 mg/mL on the surface of the modified electrode, and naturally airing at room temperature in a dark place; a photosensitive electrode for detecting tetracycline is prepared.
Example 3 preparation of photoelectrochemical sensor
（1）AgBiS 2 Preparation of nanoflower
Dissolving 0.5 g silver nitrate, 0.7 g bismuth chloride and 0.6 g L-cysteine in 50 mL N, N-dimethylformamide, stirring at room temperature for 3 h, transferring the solution into a high-pressure reaction kettle, reacting at 220 ℃ for 16 h, centrifuging and washing the obtained product with absolute ethanol and ultrapure water after the reaction is finished, and vacuum drying at 65 ℃ to obtain AgBiS 2 A nanoflower;
(2) Preparation of indium sulfide nanomaterial
Dissolving 0.7 g sodium sulfate nonahydrate and 0.5 g indium nitrate hydrate into 80 ultrapure water mL, stirring uniformly at room temperature, transferring the solution into a high-pressure reaction kettle, reacting at 220 ℃ for 16 h, cooling to room temperature after the reaction is finished, washing the obtained black product with the ultrapure water and absolute ethyl alcohol, and vacuum drying at 80 ℃ to obtain indium sulfide nanometer;
(3) Preparation of photoelectrochemical sensor
1) Ultrasonically cleaning conductive glass sequentially by using a surfactant, acetone, ethanol and ultrapure water, introducing nitrogen gas into a 70 ℃ oven for drying;
2) 25 mu L of AgBiS with concentration of 10 mg/mL is taken 2 Dripping the aqueous solution on the conductive surface of the ITO conductive glass, and baking under an infrared lamp;
3) Continuously dripping 20 mu L of indium sulfide aqueous solution with the concentration of 5 mg/mL on the surface of the modified electrode, and naturally airing at room temperature in a dark place; a photosensitive electrode for detecting tetracycline is prepared.
Example 4 detection of Tetracycline
(1) Using an electrochemical workstation to test by using a three-electrode system, wherein a saturated calomel electrode is used as a reference electrode, a platinum electrode is used as an auxiliary electrode, and the prepared ITO modified photosensitive electrode is used as a working electrode, and is tested in a PBS buffer solution with pH of 5.0 and containing 0.05-300 nmol/L glutathione;
(2) Detecting tetracycline by time-current method, setting voltage to-0.1 and V, running time to 120 s, and light source wavelength to 400 nm;
(3) After the electrodes are placed, the lamp is turned on every 10 s to continuously irradiate 10 s, record photocurrent, and draw a working curve;
(4) And (3) detecting the tetracycline sample solution to be detected instead of the tetracycline standard solution.
EXAMPLE 5 detection of Tetracycline
(1) Using an electrochemical workstation to test by using a three-electrode system, wherein a saturated calomel electrode is used as a reference electrode, a platinum electrode is used as an auxiliary electrode, and the prepared ITO modified photosensitive electrode is used as a working electrode, and is tested in a PBS buffer solution with pH of 7.0 and containing 0.05-300 nmol/L glutathione;
(2) Detecting tetracycline by a time-current method, setting the voltage to be 0V, the running time to be 120 s and the light source wavelength to be 420 nm;
(3) After the electrodes are placed, the lamp is turned on every 10 s to continuously irradiate 10 s, record photocurrent, and draw a working curve;
(4) And (3) detecting the tetracycline sample solution to be detected instead of the tetracycline standard solution.
EXAMPLE 6 detection of Tetracycline
(1) Using an electrochemical workstation to test by using a three-electrode system, wherein a saturated calomel electrode is used as a reference electrode, a platinum electrode is used as an auxiliary electrode, and the prepared ITO modified photosensitive electrode is used as a working electrode, and is tested in a PBS buffer solution with pH of 7.5 and containing 0.05-300 nmol/L glutathione;
(2) Detecting tetracycline by a time-current method, setting the voltage to be-0.1V, and the running time to be 120 s, wherein the light source wavelength is 430 nm;
(3) After the electrodes are placed, the lamp is turned on every 10 s to continuously irradiate 10 s, record photocurrent, and draw a working curve;
(4) And (3) detecting the tetracycline sample solution to be detected instead of the tetracycline standard solution.
Claims (2)
1. A preparation method of a photoelectrochemical sensor for tetracycline detection comprises the following steps:
（1）AgBiS 2 preparation of nanoflower
0.1 to 0.5. 0.5 g silver nitrate, 0.3 to 0.7. 0.7 g bismuth chloride and 0 are taken.2-0.6-g L-cysteine is dissolved in 10-50 mL N, N-dimethylformamide, after stirring is carried out at room temperature for 1-3 h, the solution is transferred into a high-pressure reaction kettle to react for 10-16 h at 150-220 ℃, after the reaction is finished, the obtained product is centrifugally washed by absolute ethyl alcohol and ultrapure water, and is dried in vacuum at 35-65 ℃ to obtain AgBiS 2 A nanoflower;
(2) Preparation of indium sulfide nanomaterial
Dissolving 0.3-0.7 g sodium sulfate nonahydrate and 0.1-0.5 g indium nitrate hydrate in 30-80 mL ultrapure water, stirring uniformly at room temperature, transferring the solution into a high-pressure reaction kettle, reacting at 150-220 ℃ for 10-16 h, cooling to room temperature after the reaction is finished, washing the obtained black product with ultrapure water and absolute ethyl alcohol, and vacuum drying at 40-80 ℃ to obtain indium sulfide nanometer;
(3) Preparation of photoelectrochemical sensor
1) Ultrasonically cleaning conductive glass sequentially by using a surfactant, acetone, ethanol and ultrapure water, introducing nitrogen gas into a 70 ℃ oven for drying;
2) Taking AgBiS with concentration of 25 mu L of 5-10 mg/mL 2 Dripping the aqueous solution on the conductive surface of the ITO conductive glass, and baking under an infrared lamp;
3) Continuously dripping 20 mu L of indium sulfide aqueous solution with the concentration of 1-5 mg/mL on the surface of the modified electrode, and naturally airing the electrode at room temperature in a dark place; a photosensitive electrode for detecting tetracycline is prepared.
2. The method for detecting a photoelectrode produced by the production method according to claim 1, comprising the steps of:
(1) Using an electrochemical workstation to test by using a three-electrode system, wherein a saturated calomel electrode is used as a reference electrode, a platinum electrode is used as an auxiliary electrode, and the prepared ITO modified photosensitive electrode is used as a working electrode, and is tested in a PBS buffer solution with pH of 5.0-8.0 and containing 0.05-300 nmol/L glutathione;
(2) Detecting the tetracycline by a time-current method, setting the voltage to be-0.1V, the running time to be 120 s, and the wavelength of a light source to be 400-450 nm;
(3) After the electrodes are placed, the lamp is turned on every 10 s to continuously irradiate 10 s, record photocurrent, and draw a working curve;
(4) And (3) detecting the tetracycline sample solution to be detected instead of the tetracycline standard solution.
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