CN111766280A - Preparation method and application of photoelectrochemical immunosensor based on tin disulfide/cadmium sulfide - Google Patents

Preparation method and application of photoelectrochemical immunosensor based on tin disulfide/cadmium sulfide Download PDF

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CN111766280A
CN111766280A CN202010483184.7A CN202010483184A CN111766280A CN 111766280 A CN111766280 A CN 111766280A CN 202010483184 A CN202010483184 A CN 202010483184A CN 111766280 A CN111766280 A CN 111766280A
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amyloid
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cadmium sulfide
tin disulfide
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王萌迪
魏琴
刘雪静
贾洪英
李玉阳
任祥
吴丹
王欢
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University of Jinan
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Abstract

The invention relates to a preparation method and application of a tin disulfide/cadmium sulfide-based photoelectrochemical immunosensor, and belongs to the technical field of novel functional materials and biosensing detection. The invention takes tin disulfide/cadmium sulfide as a substrate material and visible light as a light source to obtain photocurrent; the two components of the substrate material have good energy band matching, and the photoelectric conversion efficiency is greatly improved, so that a large output signal is obtained. To be measuredβDifferent amounts of amyloid solution, resulting in the formation of different amounts of immune complexes, and thus in different degrees of photoelectric signal(ii) an effect; the sensor has high sensitivity, wide detection range and low detection limit on target objects, and can realize the detection in human serumβQuick and sensitive measurement of amyloid has great application value in clinical judgment of infection types of patients.

Description

Preparation method and application of photoelectrochemical immunosensor based on tin disulfide/cadmium sulfide
Technical Field
The invention relates to a preparation method and application of a tin disulfide/cadmium sulfide-based photoelectrochemical immunosensor, in particular to a method for preparing a sensitive detection by adopting tin disulfide/cadmium sulfide as a substrate materialβAn amyloid photoelectrochemical immunosensor, belonging to the technical field of novel functional materials and biosensing detection.
Background
βAmyloid is a polypeptide that circulates in the blood, cerebrospinal fluid and cerebral interstitial fluid, has a strong toxic effect on the cranial nerves, can damage peripheral neurons, triggers gliosis, leads to premature apoptosis; now, at the present time,βamyloid is considered as a major biomarker of alzheimer's disease.
Researchers have adopted a variety of methods to realizeβ-detection of amyloid; for example, Carneiro et al use electrochemical methods for detection (Sensors)&Actors B Chemical 239, 157-; tang et al used fluorescence immunoassay (Spectrochim. Acta A, 201, 82-87); the excitation source and the detection source of the electrochemical detection and the fluorescence detection have the same energy form, so that a large background signal is caused, and the further reduction of the detection limit is not facilitated; the excitation source of photoelectrochemistry detection is a light source, and a detection signal is an electric signal; the difference of the energy forms of the excitation signal and the detection signal causes the photoelectric detection to have very low background signals, so that the photoelectric detection can reach an extremely low detection limit; in addition, the photoelectric detection also has the characteristics of simple equipment, high sensitivity, easy miniaturization and the like, and develops into an analysis method with great application potential.
The substrate material for generating the detected electric signal plays an important role in the performance of the sensorActing; the search for a substrate material with high photoelectric conversion efficiency and stable performance has been the exploration target of researchers; in recent years, the compounding of two or more semiconductors is found to greatly improve the photoelectric conversion efficiency of the material and overcome the problems of photo-corrosion and the like of a single component; however, most of the composite materials need to synthesize one component in advance, and then gradually react to compound the other component; for example, Liu et al (Biosensors)&Bioelectronics 86(2016) 301-7. firstly, tin disulfide is synthesized on the multi-wall carbon nanotube, and then the compounding of cadmium sulfide is realized by a reflux method, so that the multi-wall carbon nanotube/tin disulfide/cadmium sulfide composite material is generated; although the composite material synthesized by the method has better photoelectric conversion performance, the synthesis steps are complex, time and labor are consumed, and the method is not favorable for large-area popularization and application; the tin disulfide/cadmium sulfide composite material is hydrothermally synthesized by adopting a one-step method, so that the problem of complex synthetic steps of the composite material is avoided; in addition, the invention also constructs a photoelectrochemical immunosensor by taking the tin disulfide/cadmium sulfide composite material as a photoelectric conversion material, thereby realizing the aim of pairingβSensitive detection of amyloid.
Disclosure of Invention
One of the purposes of the invention is to hydrothermally synthesize a tin disulfide material by controlling the pH value of a solution to be acidic in the presence of divalent sulfur ions;
the second purpose of the invention is to synthesize the tin disulfide/cadmium sulfide composite material by a one-step hydrothermal method and realize the application of the tin disulfide/cadmium sulfide composite material in the aspect of photoelectric conversion;
the third purpose of the invention is to prepare a photoelectrochemical immunosensor with high sensitivity, strong specificity and high detection speed by using tin disulfide/cadmium sulfide as a substrate, thereby realizing the aim of pairing under the condition of visible lightβUltrasensitive detection of amyloid.
The technical scheme of the invention is as follows:
1. a preparation method of a photoelectrochemical immunosensor based on tin disulfide/cadmium sulfide comprises the following steps:
1) cutting ITO conductive glass into 2.5 × 1.0.0 cm2AnUltrasonically cleaning for 0.5 h by using decontamination powder, acetone, ethanol and ultrapure water, and drying under nitrogen;
2) dropwise adding 6 mu L of tin disulfide/cadmium sulfide solution to a conductive surface of the ITO conductive glass, and airing at room temperature;
3) soaking the modified electrode in a thioglycollic acid solution with the concentration of 1-10 mmol/L for 0.5 h, and then cleaning with ultrapure water;
4) dropwise adding 4 mu L of mixed solution of 10-500 mmoL/L1-ethyl- (3-dimethyl amino propyl) carbodiimide hydrochloride solution and 20-200 mmoL/L N-hydroxysuccinimide solution with the volume ratio of 1:1 on the surface of the modified electrode; incubating at room temperature for 0.5 h, washing the surface of the electrode with ultrapure water, and airing at room temperature to a wet film state;
5) dropwise adding 6 mu L and 1 mu g/mLβIncubating the amyloid protein antibody solution at 4 ℃ for 1 h, washing with ultrapure water, and naturally airing to a wet film state;
6) dropwise adding 6 muL of bovine serum albumin solution with the mass fraction of 1% -3% on the surface of the modified electrode, washing the surface of the electrode with ultrapure water after 0.5 h, and airing in a refrigerator at 4 ℃ to a wet film state;
7) dropwise adding the mixture at a concentration of 6 mu L of 0.5 pg/mL-100 ng/mLβThe amyloid standard solution is incubated at the constant temperature of 4 ℃ for 4 hours, and then the surface of the electrode is rinsed by ultrapure water to prepare the detection reagentβ-an amyloid photoelectrochemical immunosensor.
2. The concentration is 1. mu.g/mL as described in 1βAmyloid antibody solution 1 mg/mL available from Nanjing Kinsley Biotechnology Ltdβ-an amyloid antibody solution diluted with phosphate buffer.
3. The concentration of the compound 1 is 0.5 pg/mL-100 ng/mLβAmyloid standard solution, 1 mg/mL available from Nanjing Kinsley Biotechnology Ltdβ-the amyloid standard solution is obtained by diluting with phosphate buffer.
4. The phosphate buffer solution as described in claim 3 was prepared by mixing 0.1 mol/L disodium hydrogen phosphate solution with 0.1 mol/L potassium dihydrogen phosphate, and adjusted to have a pH of 7.4.
5. The tin disulfide/cadmium sulfide solution of claim 1, characterized by the preparation steps of:
sequentially adding 0.1-0.9 g of stannic chloride pentahydrate, 0.1-0.9 g of cadmium acetate and 0.1-0.9 g of thiourea into 30 mL of ultrapure water, and magnetically stirring for 0.5 h; then, transferring the solution into a reaction kettle, and reacting for 10-20 h at 100-200 ℃; naturally cooling; centrifugally washing the obtained product with anhydrous ethanol and ultrapure water for 3 times respectively; vacuum drying at 60 deg.C for 10 hr; grinding to obtain a tin disulfide/cadmium sulfide material; and preparing the solution into a tin disulfide/cadmium sulfide aqueous solution with the concentration of 1-6 mg/mL.
6. The photoelectrochemical immunosensor prepared by the preparation method of 1 and based on tin disulfide/cadmium sulfide, which is used forβ-detection of amyloid, characterized in that the detection steps are as follows:
1) testing by using an electrochemical workstation and a three-electrode system, taking a saturated calomel electrode as a reference electrode and a platinum wire electrode as an auxiliary electrode, taking the prepared ITO modified electrode as a working electrode, and testing in 15 mL of phosphate buffer solution with ascorbic acid dissolved at the concentration of 0.05-0.25 mol/L and the pH value of 5.0-8.0;
2) by time-current methodβDetecting an amyloid standard solution, setting the voltage to be 0V, the operation time to be 120 s, and the light source wavelength to be 400-450 nm;
3) after the electrodes are placed, turning on the lamp every 20 s for continuously irradiating for 20 s, recording the photocurrent, and drawing a working curve;
4) by means of the device under testβAmyloid sample solution replacementβAmyloid standard solutions for detection.
Advantageous results of the invention
1. The invention successfully synthesizes the tin disulfide/cadmium sulfide composite material for the first time by adopting a one-step hydrothermal method; the high-power transmission electron microscope shows that the material is in a particle shape of 4-6 nm; x-ray photoelectron spectroscopy analysis proves the existence of four elements of tin, sulfur, carbon and cadmium in the compound; thanks to the good band matching of the two components, the synthesized tin disulfide/cadmium sulfide composite material exhibits a photocurrent response of 63 microamps, which is 8 times that of tin disulfide and 10 times that of cadmium sulfide material, in the photocurrent test as described in claims 1), 2) and 3); the successful synthesis of the material not only avoids the difficult problem of gradual compounding of the composite material, but also solves the problem of low photoelectric conversion efficiency when the tin disulfide and cadmium sulfide materials are used independently; the composite material has great application potential in the aspect of photoelectric conversion.
2. The photoelectrochemical immunosensor prepared by the invention is used forβThe detection of amyloid protein has short response time, low detection limit, wide linear range and good stability, and can realize simple, quick, high-sensitivity and specific detection; sensor pair prepared by the inventionβThe linear range of amyloid detection is 0.5 pg/mL-100 ng/mL, and the detection limit reaches 0.17 pg/mL.
Detailed description of the preferred embodiments
Embodiment 1 a method for preparing a tin disulfide/cadmium sulfide-based photoelectrochemical immunosensor:
1) cutting ITO conductive glass into 2.5 × 1.0.0 cm2Ultrasonic cleaning with cleaning powder, acetone, ethanol and ultrapure water for 0.5 h in sequence, and drying under nitrogen;
2) dropwise adding 6 mu L of tin disulfide/cadmium sulfide solution to a conductive surface of the ITO conductive glass, and airing at room temperature;
3) soaking the modified electrode in 3 mmol/L mercaptoacetic acid solution for 0.5 h, and cleaning with ultrapure water;
4) dripping 4 mu L of mixed solution of 30 mmoL/L1-ethyl- (3-dimethyl amino propyl grade) carbodiimide hydrochloride solution and 20 mmoL/L N-hydroxysuccinimide solution with the volume ratio of 1:1 on the surface of the modified electrode; incubating at room temperature for 0.5 h, washing the surface of the electrode with ultrapure water, and airing at room temperature to a wet film state;
5) dropwise adding 6 mu L and 1 mu g/mLβIncubating the amyloid protein antibody solution at 4 ℃ for 1 h, washing with ultrapure water, and naturally airing to a wet film state;
6) dropwise adding 6 muL of bovine serum albumin solution with the mass fraction of 1% on the surface of the modified electrode, flushing the surface of the electrode with ultrapure water after 0.5 h, and airing in a refrigerator at 4 ℃ to a wet film state;
7) dropwise adding the mixture at a concentration of 6 mu L of 0.5 pg/mL-100 ng/mLβThe amyloid standard solution is incubated at the constant temperature of 4 ℃ for 4 hours, and then the surface of the electrode is rinsed by ultrapure water to prepare the detection reagentβ-an amyloid photoelectrochemical immunosensor.
Embodiment 2 a method for preparing a tin disulfide/cadmium sulfide-based photoelectrochemical immunosensor comprises the following steps:
1) cutting ITO conductive glass into 2.5 × 1.0.0 cm2Ultrasonic cleaning with cleaning powder, acetone, ethanol and ultrapure water for 0.5 h in sequence, and drying under nitrogen;
2) dropwise adding 6 mu L of tin disulfide/cadmium sulfide solution to a conductive surface of the ITO conductive glass, and airing at room temperature;
3) soaking the modified electrode in thioglycollic acid solution with the concentration of 6 mmol/L for 0.5 h, and cleaning with ultrapure water;
4) dripping 4 mu L of mixed solution of 100 mmoL/L1-ethyl- (3-dimethyl amino propyl grade) carbodiimide hydrochloride solution and 50 mmoL/L N-hydroxysuccinimide solution with the volume ratio of 1:1 on the surface of the modified electrode; incubating at room temperature for 0.5 h, washing the surface of the electrode with ultrapure water, and airing at room temperature to a wet film state;
5) dropwise adding 6 mu L and 1 mu g/mLβIncubating the amyloid protein antibody solution at 4 ℃ for 1 h, washing with ultrapure water, and naturally airing to a wet film state;
6) dropwise adding 6 muL of bovine serum albumin solution with the mass fraction of 2% on the surface of the modified electrode, flushing the surface of the electrode with ultrapure water after 0.5 h, and airing in a refrigerator at 4 ℃ to a wet film state;
7) dropwise adding the mixture at a concentration of 6 mu L of 0.5 pg/mL-100 ng/mLβThe amyloid standard solution is incubated at the constant temperature of 4 ℃ for 4 hours, and then the surface of the electrode is rinsed by ultrapure water to prepare the detection reagentβ-an amyloid photoelectrochemical immunosensor.
Embodiment 3 a method for preparing a tin disulfide/cadmium sulfide-based photoelectrochemical immunosensor:
1) cutting ITO conductive glass into 2.5 × 1.0.0 cm2In turn, is usedUltrasonically cleaning dirt powder, acetone, ethanol and ultrapure water for 0.5 h, and drying under nitrogen;
2) dropwise adding 6 mu L of tin disulfide/cadmium sulfide solution to a conductive surface of the ITO conductive glass, and airing at room temperature;
3) soaking the modified electrode in 9 mmol/L mercaptoacetic acid solution for 0.5 h, and cleaning with ultrapure water;
4) dropwise adding 4 mu L of mixed solution of 400 mmoL/L1-ethyl- (3-dimethyl amino propyl grade) carbodiimide hydrochloride solution and 150 mmoL/L N-hydroxysuccinimide solution with the volume ratio of 1:1 on the surface of the modified electrode; incubating at room temperature for 0.5 h, washing the surface of the electrode with ultrapure water, and airing at room temperature to a wet film state;
5) dropwise adding 6 mu L and 1 mu g/mLβIncubating the amyloid protein antibody solution at 4 ℃ for 1 h, washing with ultrapure water, and naturally airing to a wet film state;
6) dropwise adding 6 muL of bovine serum albumin solution with the mass fraction of 3% on the surface of the modified electrode, flushing the surface of the electrode with ultrapure water after 0.5 h, and airing in a refrigerator at 4 ℃ to a wet film state;
7) dropwise adding the mixture at a concentration of 6 mu L of 0.5 pg/mL-100 ng/mLβThe amyloid standard solution is incubated at the constant temperature of 4 ℃ for 4 hours, and then the surface of the electrode is rinsed by ultrapure water to prepare the detection reagentβ-an amyloid photoelectrochemical immunosensor.
Example 4 preparation of a tin disulfide/cadmium sulfide solution:
0.6 g of stannic chloride pentahydrate, 0.5 g of cadmium acetate and 0.5 g of thiourea are sequentially added into 30 mL of ultrapure water and stirred for 30 min by magnetic force; then, transferring the solution into a reaction kettle, and reacting for 19 hours at 120 ℃; naturally cooling; centrifugally washing the obtained product with anhydrous ethanol and ultrapure water for 3 times respectively; vacuum drying at 60 deg.C for 12 h; grinding to obtain a tin disulfide/cadmium sulfide material; and is prepared into tin disulfide/cadmium sulfide aqueous solution with the concentration of 1 mg/mL.
Example 5 preparation of a tin disulfide/cadmium sulfide solution:
0.2 g of stannic chloride pentahydrate, 0.7 g of cadmium acetate and 0.5 g of thiourea are sequentially added into 30 mL of ultrapure water and stirred for 30 min by magnetic force; then, transferring the solution into a reaction kettle, and reacting for 15 hours at 180 ℃; naturally cooling; centrifugally washing the obtained product with anhydrous ethanol and ultrapure water for 3 times respectively; vacuum drying at 60 deg.C for 12 h; grinding to obtain a tin disulfide/cadmium sulfide material; and is prepared into tin disulfide/cadmium sulfide aqueous solution with the concentration of 3 mg/mL.
Example 6 preparation of a tin disulfide/cadmium sulfide solution:
0.8 g of stannic chloride pentahydrate, 0.2 g of cadmium dichloride and 0.5 g of thiourea are sequentially added into 30 mL of ultrapure water and stirred magnetically for 30 min; then, transferring the solution into a reaction kettle, and reacting for 12 hours at 160 ℃; naturally cooling; centrifugally washing the obtained product with anhydrous ethanol and ultrapure water for 3 times respectively; vacuum drying at 40 deg.C for 12 h; grinding to obtain a tin disulfide/cadmium sulfide material; and is prepared into a tin disulfide/cadmium sulfide aqueous solution with the concentration of 6 mg/mL.
Example 7βDetection of amyloid
(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 wire electrode is used as an auxiliary electrode, the prepared ITO modified electrode is used as a working electrode, and the ITO modified electrode is tested in a PBS (phosphate buffer solution) with ascorbic acid dissolved in 0.1 mol/L solution, wherein the concentration of the ascorbic acid is 15 mL and the pH value of the PBS is 5.5;
(2) by time-current methodβDetecting an amyloid standard solution, setting the voltage to be 0V, the running time to be 120 s and the light source wavelength to be 400 nm;
(3) after the electrodes are placed, turning on the lamp every 20 s for continuously irradiating for 20 s, recording the photocurrent, and drawing a working curve;
(4) by means of the device under testβAmyloid sample solution replacementβAmyloid standard solutions for detection.
Example 8βDetection of amyloid
(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 wire electrode is used as an auxiliary electrode, the prepared ITO modified electrode is used as a working electrode, and the ITO modified electrode is tested in a PBS (phosphate buffer solution) with ascorbic acid dissolved in the solution with the concentration of 0.2 mol/L and the pH value of 7.4;
(2) by time-current methodβDetecting an amyloid standard solution, setting the voltage to be 0V, the running time to be 120 s and the light source wavelength to be 450 nm;
(3) after the electrodes are placed, turning on the lamp every 20 s for continuously irradiating for 20 s, recording the photocurrent, and drawing a working curve;
(4) by means of the device under testβAmyloid sample solution replacementβAmyloid standard solutions for detection.

Claims (6)

1. A preparation method of a photoelectrochemical immunosensor based on tin disulfide/cadmium sulfide is characterized by comprising the following steps:
1) cutting ITO conductive glass into 2.5 × 1.0.0 cm2Ultrasonic cleaning with cleaning powder, acetone, ethanol and ultrapure water for 0.5 h in sequence, and drying under nitrogen;
2) dropwise adding 6 mu L of tin disulfide/cadmium sulfide solution to a conductive surface of the ITO conductive glass, and airing at room temperature;
3) soaking the modified electrode in a thioglycollic acid solution with the concentration of 1-10 mmol/L for 0.5 h, and then cleaning with ultrapure water;
4) dropwise adding 4 mu L of mixed solution of 10-500 mmoL/L1-ethyl- (3-dimethyl amino propyl) carbodiimide hydrochloride solution and 20-200 mmoL/L N-hydroxysuccinimide solution with the volume ratio of 1:1 on the surface of the modified electrode;
incubating at room temperature for 0.5 h, washing the surface of the electrode with ultrapure water, and airing at room temperature to a wet film state;
5) dropwise adding 6 mu L and 1 mu g/mLβIncubating the amyloid protein antibody solution at 4 ℃ for 1 h, washing with ultrapure water, and naturally airing to a wet film state;
6) dropwise adding 6 muL of bovine serum albumin solution with the mass fraction of 1% -3% on the surface of the modified electrode, washing the surface of the electrode with ultrapure water after 0.5 h, and airing in a refrigerator at 4 ℃ to a wet film state;
7) dropwise adding the mixture at a concentration of 6 mu L of 0.5 pg/mL-100 ng/mLβStandard solution of amyloid protein, incubating at 4 deg.C for 4h, and rinsing with ultrapure waterPolar surface, making a testβ-an amyloid photoelectrochemical immunosensor.
2. The method according to claim 1, wherein the concentration is 1. mu.g/mLβAmyloid antibody solution 1 mg/mL available from Nanjing Kinsley Biotechnology Ltdβ-an amyloid antibody solution diluted with phosphate buffer.
3. The composition of claim 1, wherein the concentration is 0.5 pg/mL-100 ng/mLβAmyloid standard solution, 1 mg/mL available from Nanjing Kinsley Biotechnology Ltdβ-the amyloid standard solution is obtained by diluting with phosphate buffer.
4. The phosphate buffer solution according to claim 3, which is prepared by mixing 0.1 mol/L disodium hydrogen phosphate solution with 0.1 mol/L potassium dihydrogen phosphate, and has a pH of 7.4.
5. The tin disulfide/cadmium sulfide solution of claim 1 prepared by the steps of:
sequentially adding 0.1-0.9 g of stannic chloride pentahydrate, 0.1-0.9 g of cadmium acetate and 0.1-0.9 g of thiourea into 30 mL of ultrapure water, and magnetically stirring for 0.5 h; then, transferring the solution into a reaction kettle, and reacting for 10-20 h at 100-200 ℃; naturally cooling; centrifugally washing the obtained product with anhydrous ethanol and ultrapure water for 3 times respectively; vacuum drying at 60 deg.C for 10 hr; grinding to obtain a tin disulfide/cadmium sulfide material; and preparing the solution into a tin disulfide/cadmium sulfide aqueous solution with the concentration of 1-6 mg/mL.
6. The method of claim 1, wherein the tin disulfide/cadmium sulfide-based photoelectrochemical immunosensor is prepared by the methodβ-detection of amyloid, characterized in that the detection steps are as follows:
1) testing by using an electrochemical workstation and a three-electrode system, taking a saturated calomel electrode as a reference electrode and a platinum wire electrode as an auxiliary electrode, taking the prepared ITO modified electrode as a working electrode, and testing in 15 mL of phosphate buffer solution with ascorbic acid dissolved at the concentration of 0.05-0.25 mol/L and the pH value of 5.0-8.0;
2) by time-current methodβDetecting an amyloid standard solution, setting the voltage to be 0V, the operation time to be 120 s, and the light source wavelength to be 400-450 nm;
3) after the electrodes are placed, turning on the lamp every 20 s for continuously irradiating for 20 s, recording the photocurrent, and drawing a working curve;
4) by means of the device under testβAmyloid sample solution replacementβAmyloid standard solutions for detection.
CN202010483184.7A 2020-06-01 2020-06-01 Preparation method and application of photoelectrochemical immunosensor based on tin disulfide/cadmium sulfide Pending CN111766280A (en)

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Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2014218466A (en) * 2013-05-09 2014-11-20 富士フイルム株式会社 Aqueous solution composition
CN106124584A (en) * 2016-06-20 2016-11-16 济南大学 A kind of based on CdS@SnS2the preparation method and application of@MWCNTs unmarked type insulin photoelectricity immunosensor
CN109142745A (en) * 2018-07-27 2019-01-04 济南大学 It is a kind of based on stannic oxide/cadmium carbonate/cadmium sulfide optical electro-chemistry immunosensor preparation method and application
CN110482594A (en) * 2019-09-12 2019-11-22 安徽工程大学 Cu2CdSnS4Micro-nano material and preparation method

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2014218466A (en) * 2013-05-09 2014-11-20 富士フイルム株式会社 Aqueous solution composition
CN106124584A (en) * 2016-06-20 2016-11-16 济南大学 A kind of based on CdS@SnS2the preparation method and application of@MWCNTs unmarked type insulin photoelectricity immunosensor
CN109142745A (en) * 2018-07-27 2019-01-04 济南大学 It is a kind of based on stannic oxide/cadmium carbonate/cadmium sulfide optical electro-chemistry immunosensor preparation method and application
CN110482594A (en) * 2019-09-12 2019-11-22 安徽工程大学 Cu2CdSnS4Micro-nano material and preparation method

Non-Patent Citations (5)

* Cited by examiner, † Cited by third party
Title
LIU YIXIN 等: "Visible-light driven photoelectrochemical immunosensor for insulin detection based on MWCNTs@ SnS2@CdS nanocomposites", 《BIOSENSORS AND BIOELECTRONICS》 *
ZHANG LEI 等: "Enhanced photocatalytic activity of CdS/SnS2 nanocomposite with highly-efficient charge transfer and visible light utilization for selective reduction of 4-nitroaniline", 《JOURNAL OF COLLOID AND INTERFACE SCIENCE》 *
ZHANG YIFENG 等: "Label-free photoelectrochemical immunosensor for amyloid β-protein detection based on SnO2/CdCO3/CdS synthesized by one-pot method", 《BIOSENSORS AND BIOELECTRONICS》 *
刘佳莉等: "基于红荧烯纳米材料构建电致化学发光免疫传感器用于灵敏检测β淀粉样蛋白的研究", 《化学传感器》 *
王玲玲等: "CdS/ZnO复合颗粒的制备与电致发光性能", 《功能材料》 *

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