CN114280123A - 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 relates to AgBiS sensitized by indium sulfide nano material2Obtaining anodic photocurrent, AgBiS, as a substrate material2The nano material 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 test electrolyte solution, so that the detection sensitivity is effectively improved, and the sensitive detection of the tetracycline is realized. The detection limit is 0.022 nmol/L.
Description
Technical Field
The invention relates to a preparation method of a photoelectrochemical sensor for tetracycline detection. In particular to an AgBiS sensitized by indium sulfide2The nanoflower is used as a substrate photosensitive material to obtain anode photocurrent, and tetracycline to be detected is directly dissolved in a test electrolyte solution to prepare the photoelectrochemical sensor for sensitively detecting the tetracycline, and the photoelectrochemical sensor belongs to the technical field of novel functional materials and sensing detection.
Background
The tetracycline hydrochloride is a broad-spectrum antibiotic, has an inhibiting effect on most gram-positive and gram-negative bacteria, has a bactericidal effect at a high concentration, can inhibit rickettsia, trachoma virus and the like, and has a good effect on gram-negative bacilli. The action mechanism is mainly to prevent aminoacyl from being combined with ribonucleoprotein body, prevent peptide chain from growing and protein from synthesizing, thereby inhibiting the growth of bacteria, and have bactericidal action at high concentration. Tetracyclines are antibiotics widely used in veterinary and human therapy. Tetracyclines may be present in food products because they are overused in veterinary medicine as growth promoters and antibiotics. The residues of these antibiotics in food products can have adverse effects on human health and bacterial resistance to tetracycline antibiotics occurs in humans and veterinary medicine. Liver damage, allergic reactions and tooth yellowing are common side effects of tetracycline. Therefore, sensitive and specific methods for detecting tetracyclines in serum and food are necessary. Common methods for detecting glutathione include fluorescence analysis, colorimetric analysis, electrochemical analysis, and the like. However, the fluorescence analysis method is often complex 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 tetracycline, the analysis speed is high, the operation is simple, the stability is good, and the detection limit of the photoelectrochemical sensor designed by the invention to the tetracycline reaches 0.022 nmol/L.
AgBiS2The semiconductor nano material has good photocatalytic performance and photoelectric performance, is simple in preparation method, non-toxic, and has certain photostability and thermal stability, photo-generated charges can be generated under the irradiation of visible light, and then photocurrent is formed, but due to the narrow band gap width, photo-generated electrons and holes can be rapidly compounded after the visible light is excited, so that the utilization rate of the visible light is greatly reduced. Indium sulfide is used as an excellent sensitizing material, and has the advantages of simple preparation, high yield and good stability. Nano flower-shaped AgBiS2The specific surface area of the glass is large, and a large amount of AgBiS2 can be loaded by sensitizing the glass by indium sulfide, so that excellent photoelectric property is obtained. Directly dissolving tetracycline to be tested in photoelectrochemical testIn the electrolyte solution, the electrolyte solution 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 electron donor, so that the detection sensitivity of the sensor is improved, and the detection sensitivity of the sensor is greatly improved.
A photoelectrochemical sensor is a type of detection device that determines the concentration of an analyte based on the photoelectric conversion characteristics of a substance. The photoelectrochemical detection method has the characteristics of simple equipment, high sensitivity and easiness in miniaturization, has been developed into an analysis method with great application potential, and has wide application prospects in the fields of food, environment, medicine and the like. Indium sulfide sensitized AgBiS2The application of the nano material in the aspect of the photoelectrochemical sensor is not reported. The invention relates to AgBiS based on indium sulfide sensitization2The nano material successfully constructs a photoelectrochemical sensor for detecting tetracycline under visible light. The sensor is indium sulfide sensitized nano flower-shaped AgBiS2As a substrate photosensitive material, tetracycline to be detected is directly dissolved in a test electrolyte solution, so that sensitive detection of the tetracycline is realized. 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 rapid and high-sensitivity detection of glutathione in a visible light region, and effectively overcomes the defects of the prior tetracycline detection method.
Disclosure of Invention
One of the objects of the present invention is AgBiS sensitized with indium sulfide2The nanoflower material is used as a photosensitive material. The photosensitive material has excellent photoelectric property and has extremely high photoelectric conversion efficiency under visible light.
The other purpose of the invention is to directly dissolve the tetracycline to be detected in the test base solution, so that the detection sensitivity is greatly improved.
The third purpose of the invention is to use indium sulfide-AgBiS2The nano material is used as a substrate, the photoelectric chemical sensor with high sensitivity, good stability and high detection speed is prepared, and the aim of sensitively detecting tetracycline under the visible light condition 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）AgBiS2preparation of nanoflower
Dissolving 0.1-0.5 g of silver nitrate, 0.3-0.7 g of bismuth chloride and 0.2-0.6 g of L-cysteine in 10-50 mL of N, N-dimethylformamide, stirring at room temperature for 1-3 h, transferring the solution into a high-pressure reaction kettle, reacting at 150-220 ℃ for 10-16 h, after the reaction is finished, centrifugally washing the obtained product with absolute ethyl alcohol and ultrapure water, and drying at 35-65 ℃ in vacuum to obtain the AgBiS2A nanoflower;
(2) preparation of indium sulfide nano material
Dissolving 0.3-0.7 g of sodium sulfate nonahydrate and 0.1-0.5 g of indium nitrate hydrate in 30-80 mL of 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 drying in vacuum at 40-80 ℃ to obtain indium sulfide nano particles;
(3) preparation of photoelectrochemical sensor
1) Ultrasonically cleaning conductive glass by sequentially using a surfactant, acetone, ethanol and ultrapure water, introducing nitrogen, and drying in a 70 ℃ oven;
2) taking AgBiS with 25 mu L concentration of 5-10 mg/mL2Dripping the aqueous solution on the conductive surface of the ITO conductive glass, and drying under an infrared lamp;
3) continuously dropwise adding 20 muL of indium sulfide aqueous solution with the concentration of 1-5 mg/mL on the surface of the modified electrode, and naturally airing in a dark place at room temperature; and preparing the photosensitive electrode for detecting tetracycline.
2. The method for detecting a photosensitive electrode prepared by the preparation method according to claim 1, comprising the steps of:
(1) an electrochemical workstation is used for testing by a three-electrode system, a saturated calomel electrode is used as a reference electrode, a platinum electrode is used as an auxiliary electrode, the prepared ITO modified photosensitive electrode is used as a working electrode, and the test is carried out in 10 mL of PBS (phosphate buffer solution) containing 0.05-300 nmol/L of glutathione and having the pH value of 5.0-8.0;
(2) detecting tetracycline by a time-current method, setting the voltage to be-0.1V, the operation time to be 120 s, and the wavelength of a light source to be 400-450 nm;
(3) after the electrodes are placed, turning on the lamp every 10 s for continuously irradiating for 10 s, recording the photocurrent, and drawing a working curve;
(4) and replacing the tetracycline sample solution to be detected with the tetracycline standard solution for detection.
The linear range of the tetracycline detection of the sensor is 0.05-300 nmol/L, and the detection limit is 0.022 nmol/L.
The chemicals required for material synthesis were all purchased from local reagent stores and were not reprocessed.
Advantageous results of the invention
(1) The invention successfully synthesizes the flower-shaped AgBiS with certain photoelectric property2The nano material has low preparation cost, no toxicity and large specific surface area; AgBiS by good sensitization of indium sulfide2Sensitization is carried out, excellent photoelectric performance is obtained, and the problem of simple AgBiS is solved2And the problem of low photoelectric conversion efficiency of pure indium sulfide.
(2) The invention directly dissolves the object to be detected in the photoelectrochemistry test electrolyte solution, and the photoelectric signal is gradually increased along with the increase of the concentration of the object to be detected, thereby realizing the sensitive detection of the tetracycline.
(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, quick, high-sensitivity and specific detection. The linear range of the detection of the tetracycline is 0.05-300 nmol/L, and the detection limit is 0.022 nmol/L.
Detailed description of the preferred embodiments
EXAMPLE 1 preparation of photoelectrochemical sensor
（1）AgBiS2Preparation of nanoflower
Dissolving 0.1 g of silver nitrate, 0.3 g of bismuth chloride and 0.2 g of L-cysteine in 10 mL of N, N-dimethylformamide, stirring at room temperature for 1 h, and transferring the solution into a high-pressure reaction kettleReacting at 150 ℃ for 10 h, after the reaction is finished, centrifugally washing the obtained product by using absolute ethyl alcohol and ultrapure water, and drying in vacuum at 35 ℃ to obtain AgBiS2A nanoflower;
(2) preparation of indium sulfide nano material
Dissolving 0.3 g of sodium sulfate nonahydrate and 0.1 g of indium nitrate hydrate in 30 mL of ultrapure water, stirring uniformly at room temperature, transferring the solution into a high-pressure reaction kettle, reacting at 150 ℃ for 10 hours, cooling to room temperature after the reaction is finished, washing the obtained black product with ultrapure water and absolute ethyl alcohol, and drying in vacuum at 40 ℃ to obtain indium sulfide nano-particles;
(3) preparation of photoelectrochemical sensor
1) Ultrasonically cleaning conductive glass by sequentially using a surfactant, acetone, ethanol and ultrapure water, introducing nitrogen, and drying in a 70 ℃ oven;
2) taking AgBiS with 25 mu L concentration of 5 mg/mL2Dripping the aqueous solution on the conductive surface of the ITO conductive glass, and drying under an infrared lamp;
3) continuously dropwise adding 20 muL of indium sulfide aqueous solution with the concentration of 1 mg/mL on the surface of the modified electrode, and naturally airing in a dark place at room temperature; and preparing the photosensitive electrode for detecting tetracycline.
EXAMPLE 2 preparation of photoelectrochemical sensor
（1）AgBiS2Preparation of nanoflower
Dissolving 0.1-0.5 g of silver nitrate, 0.3-0.7 g of bismuth chloride and 0.2-0.6 g of L-cysteine in 10-50 mL of N, N-dimethylformamide, stirring at room temperature for 1-3 h, transferring the solution into a high-pressure reaction kettle, reacting at 150-220 ℃ for 10-16 h, after the reaction is finished, centrifugally washing the obtained product with absolute ethyl alcohol and ultrapure water, and drying at 35-65 ℃ in vacuum to obtain the AgBiS2A nanoflower;
(2) preparation of indium sulfide nano material
Dissolving 0.5 g of sodium sulfate nonahydrate and 0.3 g of indium nitrate hydrate in 50 mL of ultrapure water, stirring uniformly at room temperature, transferring the solution into a high-pressure reaction kettle, reacting at 160 ℃ for 12 hours, cooling to room temperature after the reaction is finished, washing the obtained black product with ultrapure water and absolute ethyl alcohol, and drying in vacuum at 60 ℃ to obtain indium sulfide nano-particles;
(3) preparation of photoelectrochemical sensor
1) Ultrasonically cleaning conductive glass by sequentially using a surfactant, acetone, ethanol and ultrapure water, introducing nitrogen, and drying in a 70 ℃ oven;
2) taking AgBiS with 25 mu L concentration of 6 mg/mL2Dripping the aqueous solution on the conductive surface of the ITO conductive glass, and drying under an infrared lamp;
3) continuously dropwise adding 20 muL of indium sulfide aqueous solution with the concentration of 2 mg/mL on the surface of the modified electrode, and naturally airing in a dark place at room temperature; and preparing the photosensitive electrode for detecting tetracycline.
EXAMPLE 3 preparation of photoelectrochemical sensor
（1）AgBiS2Preparation of nanoflower
Dissolving 0.5 g of silver nitrate, 0.7 g of bismuth chloride and 0.6 g of L-cysteine in 50 mL of 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, centrifugally washing the obtained product with absolute ethyl alcohol and ultrapure water after the reaction is finished, and drying in vacuum at 65 ℃ to obtain AgBiS2A nanoflower;
(2) preparation of indium sulfide nano material
Dissolving 0.7 g of sodium sulfate nonahydrate and 0.5 g of indium nitrate hydrate in 80 mL of ultrapure water, 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 ultrapure water and absolute ethyl alcohol, and drying in vacuum at 80 ℃ to obtain indium sulfide nano-particles;
(3) preparation of photoelectrochemical sensor
1) Ultrasonically cleaning conductive glass by sequentially using a surfactant, acetone, ethanol and ultrapure water, introducing nitrogen, and drying in a 70 ℃ oven;
2) taking AgBiS with 25 mu L concentration of 10 mg/mL2Dripping the aqueous solution on the conductive surface of the ITO conductive glass, and drying under an infrared lamp;
3) continuously dropwise adding 20 muL of indium sulfide aqueous solution with the concentration of 5 mg/mL on the surface of the modified electrode, and naturally airing in a dark place at room temperature; and preparing the photosensitive electrode for detecting tetracycline.
Example 4 detection of Tetracycline
(1) Testing by using an electrochemical workstation in a three-electrode system, taking a saturated calomel electrode as a reference electrode and a platinum electrode as an auxiliary electrode, taking the prepared ITO modified photosensitive electrode as a working electrode, and testing in 10 mL of PBS (phosphate buffer solution) containing 0.05-300 nmol/L of glutathione and having the pH value of 5.0;
(2) detecting 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 nm;
(3) after the electrodes are placed, turning on the lamp every 10 s for continuously irradiating for 10 s, recording the photocurrent, and drawing a working curve;
(4) and replacing the tetracycline sample solution to be detected with the tetracycline standard solution for detection.
EXAMPLE 5 detection of Tetracycline
(1) Testing by using an electrochemical workstation in a three-electrode system, taking a saturated calomel electrode as a reference electrode and a platinum electrode as an auxiliary electrode, taking the prepared ITO modified photosensitive electrode as a working electrode, and testing in 10 mL of PBS (phosphate buffer solution) containing 0.05-300 nmol/L of glutathione and having the pH value of 7.0;
(2) detecting tetracycline by a time-current method, setting the voltage to be 0V, the operation time to be 120 s, and the light source wavelength to be 420 nm;
(3) after the electrodes are placed, turning on the lamp every 10 s for continuously irradiating for 10 s, recording the photocurrent, and drawing a working curve;
(4) and replacing the tetracycline sample solution to be detected with the tetracycline standard solution for detection.
EXAMPLE 6 detection of Tetracycline
(1) Testing by using an electrochemical workstation in a three-electrode system, taking a saturated calomel electrode as a reference electrode and a platinum electrode as an auxiliary electrode, taking the prepared ITO modified photosensitive electrode as a working electrode, and testing in 10 mL of PBS (phosphate buffer solution) containing 0.05-300 nmol/L of glutathione and having the pH value of 7.5;
(2) detecting tetracycline by a time-current method, setting the voltage to be-0.1V, the operation time to be 120 s, and the light source wavelength to be 430 nm;
(3) after the electrodes are placed, turning on the lamp every 10 s for continuously irradiating for 10 s, recording the photocurrent, and drawing a working curve;
(4) and replacing the tetracycline sample solution to be detected with the tetracycline standard solution for detection.
Claims (2)
1. A preparation method of a photoelectrochemical sensor for tetracycline detection comprises the following steps:
（1）AgBiS2preparation of nanoflower
Dissolving 0.1-0.5 g of silver nitrate, 0.3-0.7 g of bismuth chloride and 0.2-0.6 g of L-cysteine in 10-50 mL of N, N-dimethylformamide, stirring at room temperature for 1-3 h, transferring the solution into a high-pressure reaction kettle, reacting at 150-220 ℃ for 10-16 h, after the reaction is finished, centrifugally washing the obtained product with absolute ethyl alcohol and ultrapure water, and drying at 35-65 ℃ in vacuum to obtain the AgBiS2A nanoflower;
(2) preparation of indium sulfide nano material
Dissolving 0.3-0.7 g of sodium sulfate nonahydrate and 0.1-0.5 g of indium nitrate hydrate in 30-80 mL of 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 drying in vacuum at 40-80 ℃ to obtain indium sulfide nano particles;
(3) preparation of photoelectrochemical sensor
1) Ultrasonically cleaning conductive glass by sequentially using a surfactant, acetone, ethanol and ultrapure water, introducing nitrogen, and drying in a 70 ℃ oven;
2) taking AgBiS with 25 mu L concentration of 5-10 mg/mL2Dripping the aqueous solution on the conductive surface of the ITO conductive glass, and drying under an infrared lamp;
3) continuously dropwise adding 20 muL of indium sulfide aqueous solution with the concentration of 1-5 mg/mL on the surface of the modified electrode, and naturally airing in a dark place at room temperature; and preparing the photosensitive electrode for detecting tetracycline.
2. The method for detecting a photosensitive electrode prepared by the preparation method according to claim 1, comprising the steps of:
(1) an electrochemical workstation is used for testing by a three-electrode system, a saturated calomel electrode is used as a reference electrode, a platinum electrode is used as an auxiliary electrode, the prepared ITO modified photosensitive electrode is used as a working electrode, and the test is carried out in 10 mL of PBS (phosphate buffer solution) containing 0.05-300 nmol/L of glutathione and having the pH value of 5.0-8.0;
(2) detecting tetracycline by a time-current method, setting the voltage to be-0.1V, the operation time to be 120 s, and the wavelength of a light source to be 400-450 nm;
(3) after the electrodes are placed, turning on the lamp every 10 s for continuously irradiating for 10 s, recording the photocurrent, and drawing a working curve;
(4) and replacing the tetracycline sample solution to be detected with the tetracycline standard solution for detection.
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