CN113252752B - Preparation method of sulfur nanoparticle/MOF/boron nanosheet/ferrocenyl nano hybrid ratio electrochemical sensor - Google Patents
Preparation method of sulfur nanoparticle/MOF/boron nanosheet/ferrocenyl nano hybrid ratio electrochemical sensor Download PDFInfo
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- G—PHYSICS
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
- G01N27/26—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating electrochemical variables; by using electrolysis or electrophoresis
- G01N27/28—Electrolytic cell components
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
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- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B17/00—Sulfur; Compounds thereof
- C01B17/02—Preparation of sulfur; Purification
- C01B17/06—Preparation of sulfur; Purification from non-gaseous sulfides or materials containing such sulfides, e.g. ores
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B35/00—Boron; Compounds thereof
- C01B35/02—Boron; Borides
- C01B35/023—Boron
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G83/00—Macromolecular compounds not provided for in groups C08G2/00 - C08G81/00
- C08G83/008—Supramolecular polymers
Abstract
The invention discloses a preparation method of a sulfur nanoparticle SNPs/metal organic framework MOF compound/boron nanosheet BNSs/ferrocene Fc-based nano hybrid ratio electrochemical sensor, which comprises the steps of respectively preparing SNPs, SNPs@MOF hybrids encapsulated in the SNPs, BNSs and BNSS-Fc complexes, gradually dripping BNSS-Fc and SNPs@MOF on the surface of a glassy carbon electrode GCE, preparing a SNPs@MOF/BNSS-Fc nano hybrid modified GCE electrochemical sensing interface, taking the modified electrode as a working electrode, adding doxorubicin ADR in electrolyte, measuring an electrochemical square wave voltammetry curve under different coexistence concentrations of the ADR by adopting an electrochemical workstation, fitting a linear relation between the current intensity ratio of the ADR and an Fc redox peak and the corresponding ADR concentration, and constructing the ratio electrochemical sensor for high-efficiency detection of the ADR.
Description
Technical Field
The invention belongs to the technical field of preparation of Metal Organic Framework (MOF) hybrids, boron nano-sheet composites and ratio electrochemical sensors, and particularly relates to a preparation method of a ratio electrochemical sensor based on sulfur nano-particles/MOF/boron nano-sheets/ferrocene nano-hybrids.
Background
In the periodic table of chemical elements, boron is adjacent to beryllium and carbon, having similar metallic properties andnonmetallic compounds are abundant in variety with a variety of elements by forming conventional covalent bonds and multicenter chemical bonds. The crystal structure of boron reaches hundreds of species, wherein bulk phase crystal boron mostly contains B 12 Icosahedral structural units, but a few contain gamma-rhombic boron dumbbell-shaped B 2 A unit. In the field of nano science, the boron nano material has properties which are distinct from those of bulk phase materials, and can form a planar structure similar to benzene ring organic molecules and a nano structure similar to cage, tube, film and the like of fullerene. Theoretical prediction and experimental research show that the boron alkene and few-layer boron nano sheet has unique properties including two-dimensional metallicity, elasticity, flexibility, optical transparency, electronic characteristics and the like, and has application prospects in the fields of energy storage, superconduction, sensors, flexible electronics, optoelectronic devices and the like. Ultra-thin boron nanoplatelets are prepared by an ultrasonic-assisted liquid phase exfoliation method from DingtaoMa et al as novel two-dimensional luminescent materials for cell bioimaging (DingtaoMa, jinlai Zhao, jianlei Xie, feng Zhang, rui Wang, leimng Wu, weiyuan Liang, delong Li, yanqi Ge, jianqing Li, yuteng Zhang, han Zhang, ultrathin boron nanosheets as an emerging two-dimensional photoluminescence material for bioimaging, nanoscale Horizons, 2020,5,705-713).
Metal-organic framework (MOF) compounds are a class of crystalline porous materials with periodic network structures formed by self-assembly of Metal ions or Metal clusters of inorganic Metal centers with bridged organic ligands. MOF is not only an organic/inorganic hybrid material, but also a coordination polymer, and has the rigidity of inorganic materials and the flexibility of organic materials. In view of the performances of MOF such as porosity, large specific surface area, multi-metal sites and the like, the method has great development potential in the field of modern material research, and particularly has wide application prospects in important fields such as adsorption, storage, separation, sensing, catalysts, porous materials, magnetic materials, optical materials, medicine slow release and the like. Wang Peilong A gallium metal organic framework material and its sensing application in detecting endocrine disruptors are disclosed (Wang Peilong; yang Haosen; su Xiaoou; wang Ruiguo; cheng; zhang Su; dong Shujun. National invention patent, application publication No. CN 109507317A). Jin Chuanming et al disclose a paranitroaromatic explosive sensing anion framework metal organic framework material and a preparation method and application thereof (Jin Chuanming; zhou Junjiang; du Xiaogang; chen Yu; zhangpeng. National invention patent, application publication number: CN 110358106A).
The invention discloses a preparation method of a ratio electrochemical sensor based on a Boron nano-sheet compound and MOF hybrids, which designs and prepares a Boron nano-sheet/Ferrocene (BNSS-Fc) compound, SNPs@MOF hybrids encapsulated in sulfur nano-particles (Sulfur nanoparticles, SNPs), and the SNPs@MOF and BNSS-Fc are gradually dripped on the surface of a glassy carbon electrode GCE to prepare an electrochemical sensing interface of the SNPs@MOF/BNSS-Fc/GCE modified electrode. In the electrolyte solution, the externally added adriamycin ADR generates oxidation reduction at the electrochemical sensing interface, and the electrochemical oxidation reduction signal is obviously enhanced along with the increase of the ADR concentration; the ferrocene Fc is loaded in the SNPs@MOF/BNSS-Fc nanometer hybrid, and the redox signal of the ferrocene Fc is kept unchanged, so that the ferrocene Fc can be used as a reference signal. Therefore, a ratio electrochemical sensor is constructed based on SNPs@MOF/BNSs-Fc/GCE sensing interface for efficient detection of ADR. At present, domestic and foreign literature and patent reports of SNPs@MOF/BNSS-Fc nanometer hybrids and related research work of a ratio electrochemical sensing interface are not searched.
Disclosure of Invention
The invention aims to develop a preparation method of a novel, simple and efficient sulfur nanoparticle/MOF/boron nanosheet/ferrocenyl nano hybrid ratio electrochemical sensor, which can be used for efficiently detecting antibiotic medicine Adriamycin (ADR) in biological fluid samples.
In order to achieve the above object, the present invention relates to a sulfur nanoparticle/MOF/boron nanosheet/ferrocenyl nanoshutch ratio electrochemical sensor, the preparation method of which comprises the steps of:
(1) Dissolving sodium sulfide and sublimed sulfur powder in distilled water DDW, and stirring to obtain sodium polysulfide Na 2 S x Adding polyethylene glycol PEG-400 into the solution to form a mixed solution-1; dissolving formic acid and PEG-400 in distilled water DDW, and stirring to obtain mixed solution-2; dropwise adding the mixed solution-1 into the mixed solution-2, and fully stirring to form a product mixed solution-3; centrifugally separating a product mixed solution-3, washing the obtained precipitate with n-hexane for three times, then washing with ethanol, and carrying out vacuum drying treatment to obtain dried sulfur nanoparticle SNPs powder;
(2) Preparing ethanol solution-1 in which cobalt nitrate hexahydrate is dissolved, and preparing ethanol solution-2 in which 2-methylimidazole is dissolved; adding SNPs powder and polyvinylpyrrolidone PVP into an empty beaker, sequentially adding an ethanol solution-1 and an ethanol solution-2 into the SNPs powder and polyvinylpyrrolidone PVP under sufficient stirring, and performing stirring reaction on the formed mixed solution for a period of time at room temperature; centrifugally separating the product solution after the reaction is finished, washing the product solution for three times by adopting ethanol, and carrying out vacuum drying treatment to obtain SNPs@MOF hybrid powder encapsulated in the dried SNPs, so as to prepare ethanol dispersion;
(3) Preparing a few-layer boron nano-sheets BNSs by adopting an ultrasonic-assisted liquid phase stripping method, preparing ethanol dispersion liquid of the BNSs, then dropwise adding a chloroform solution in which ferrocene Fc is dissolved, and forming ethanol-chloroform dispersion liquid of BNSFc complex under sufficient stirring for standby;
(4) Dropwise adding Nafion solution on the surface of a clean glassy carbon electrode GCE, dropwise adding 1-5 drops of ethanol-chloroform dispersion liquid of BNSS-Fc complex, dropwise adding 1-5 drops of ethanol dispersion liquid of SNPs@MOF hybrid, drying one drop of ethanol dispersion liquid under nitrogen flow after each drop, and finally preparing SNPs@MOF/BNSS-Fc self-assembled nano hybrid modified GCE, wherein the SNPs@MOF/BNSS-Fc self-assembled nano hybrid modified GCE is used as an electrochemical sensing interface;
(5) Inserting SNPs@MOF/BNSs-Fc/GCE serving as a working electrode into an electrolytic cell, taking Ag/AgCl as a reference electrode, taking a platinum wire as a counter electrode, taking phosphate buffer salt solution as electrolyte, adding DDW solution in which adriamycin ADR is dissolved, measuring electrochemical square wave voltammetry curves under different coexisting concentrations of ADR by adopting a three-electrode system of an electrochemical workstation, and fitting the oxidation-reduction peak current intensity ratio I of the ADR and Fc ADR /I Fc Constructing a ratio electrochemical sensor based on SNPs@MOF/BNSs-Fc/GCE modified electrode sensing interface with the corresponding ADR coexisting concentration in a linear relation for efficiently detecting the adriamycin ADR, wherein the ADR concentrationThe linear detection range is 0.01-10 micromoles/liter, and the detection limit is 0.01-0.1 micromoles/liter.
The invention has the effect of disclosing a preparation method of a sulfur nanoparticle/MOF/boron nanosheet/ferrocenyl nano hybrid ratio electrochemical sensor. The SNPs of sulfur nano particles stabilized by polyethylene glycol PEG-400 are synthesized by adopting a water phase, polyvinylpyrrolidone PVP is used as an SNPs coating agent, cobalt nitrate hexahydrate and 2-methylimidazole are used as MOF precursors, and SNPs@MOF hybrids encapsulated in the SNPs are synthesized in ethanol at room temperature. And preparing boron nano-sheets BNSs by adopting an ultrasonic-assisted liquid phase stripping method, and adding chloroform dispersion liquid of ferrocene Fc into ethanol dispersion liquid of BNSs to prepare BNSs-Fc complex. And (3) gradually dripping BNSS-Fc complex and SNPs@MOF hybrids on the surface of the glassy carbon electrode GCE to prepare an electrochemical sensing interface of the SNPs@MOF/BNSS-Fc/GCE modified electrode. The modified electrode is used as a working electrode, phosphate buffer salt solution is used as electrolyte, adriamycin ADR aqueous dispersion is added, and electrochemical square wave voltammograms under different ADR coexistence concentrations are measured by an electrochemical workstation. Its electrochemical redox signal increases significantly as the ADR concentration increases, as a response signal. Fc was loaded in SNPs@MOF/BNSS-Fc nanohybrids, with the redox signal remaining unchanged as a reference signal. Fitting ADR and Fc redox peak amperage ratio I ADR /I Fc And a ratio electrochemical sensor is constructed based on the SNPs@MOF/BNSs-Fc/GCE sensing interface and is used for high-efficiency detection of ADR.
Drawings
FIG. 1 is a schematic diagram of a preparation method and a working principle of a sulfur nanoparticle/MOF/boron nanosheet/ferrocenyl nanoshutch ratio electrochemical sensor.
Detailed Description
The invention will now be described in detail by means of specific embodiments thereof with reference to the accompanying drawings.
Example 1
The schematic diagrams of the preparation method and the working principle of the sulfur nanoparticle/MOF/boron nanosheet/ferrocenyl nanosize hybrid ratio electrochemical sensor related to the embodiment are shown in fig. 1, and the specific preparation steps are as follows:
78mg will be 78mgDissolving sodium sulfide and 32mg of sublimed sulfur powder in 50mL of double distilled water DDW, and stirring for 24h to form sodium polysulfide Na 2 S x A solution; 10mLNa was measured 2 S x Adding 5mL of polyethylene glycol PEG-400 and 35mL of LDDW into the solution, and uniformly stirring to form a mixed solution-1; adding 10mL 2mol/L formic acid aqueous solution and 10mL PEG-400 into 30mL LDDW, and uniformly stirring to form mixed solution-2; dropwise adding the mixed solution-1 into the mixed solution-2, and stirring for 30min to form a product mixed solution; centrifuging at 5000rpm for 15min, washing the precipitate with n-hexane for three times, washing with ethanol, and vacuum drying to obtain dry sulfur nanoparticle SNPs powder.
53mg of cobalt nitrate hexahydrate is dissolved in 25mL of ethanol and stirred uniformly to form a solution-1; 66mg of 2-methylimidazole is dissolved in 25mL of ethanol and stirred uniformly to form solution-2; adding 64mg of SNPs powder and 10mg of polyvinylpyrrolidone PVP into an empty beaker, sequentially adding the solution-1 and the solution-2 into the mixture under sufficient stirring, and performing stirring reaction for 24 hours at room temperature; and (3) centrifuging the product solution after the reaction is finished at 3500rpm for 10min, washing the obtained precipitate with ethanol for three times, and performing vacuum drying treatment to obtain SNPs@MOF hybrid powder encapsulated in the dried SNPs. An ethanol dispersion of SNPs@MOF was prepared for use, wherein the concentration of SNPs@MOF was 2mg/mL.
Adding 54mg of boron powder into 20mL of isopropanol, stirring uniformly, performing ultrasonic treatment for 20min by using a probe, performing ultrasonic treatment for 24h in a water bath, centrifuging the mixed solution at 3500rpm for 20min, taking the upper mixed solution, centrifuging at 10000rpm for 10min, washing the obtained precipitate with ethanol and DDW for three times, and performing vacuum drying treatment to obtain the boron nano-sheet BNSs. An ethanol dispersion of BNSs was prepared, and a chloroform solution of ferrocene Fc was added dropwise with stirring to form an ethanol-chloroform dispersion of BNSFc complex, wherein BNSs concentration was 5mg/mL and Fc concentration was 2mmol/L.
Dripping 5 mu L of 0.5% Nafion ethanol solution on the surface of a clean glassy carbon electrode GCE, then dropwise adding 2 drops of BNSS-Fc dispersion liquid, dropwise adding 1 drop of SNPs@MOF dispersion liquid, drying under nitrogen flow after each drop, and dripping one drop to obtain SThe NPs@MOF/BNSs-Fc/GCE modifies the electrochemical sensing interface of the electrode. Inserting the modified electrode serving as a working electrode into an electrolytic tank, taking Ag/AgCl as a reference electrode, taking a platinum wire as a counter electrode, taking phosphate buffer salt solution as electrolyte, adding DDW solution in which adriamycin ADR is dissolved, measuring electrochemical square wave voltammetry curves under different coexisting concentrations of the ADR by adopting a three-electrode system of an electrochemical workstation, and fitting the oxidation-reduction peak current intensity ratio I of the ADR and Fc ADR /I Fc And constructing a ratio electrochemical sensor based on SNPs@MOF/BNSs-Fc/GCE modified electrode sensing interface with the corresponding ADR coexistence concentration in a linear relation, and using the ratio electrochemical sensor to efficiently detect the adriamycin ADR, wherein the linear detection range of the ADR concentration is 0.01-1 micromole/liter, and the detection limit is 0.01 micromole/liter.
Example 2
The schematic diagrams of the preparation method and the working principle of the sulfur nanoparticle/MOF/boron nanosheet/ferrocenyl nanosize hybrid ratio electrochemical sensor related to the embodiment are shown in fig. 1, wherein the preparation of sulfur nanoparticle SNPs, SNPs encapsulated in SNPs@MOF hybrids, boron nanosize BNSs and BNSS-Fc complexes is the same as that of embodiment 1, and other specific preparation steps are as follows:
and 5 mu L of 0.5% Nafion ethanol solution is dripped on the surface of a clean glassy carbon electrode GCE, 3 drops of BNSS-Fc dispersion liquid are added dropwise, 2 drops of SNPs@MOF dispersion liquid are added dropwise, one drop is added dropwise, and the SNPs@MOF/BNSS-Fc/GCE modified electrode electrochemical sensing interface is prepared by drying under nitrogen flow and dripping one drop. Inserting the modified electrode serving as a working electrode into an electrolytic tank, taking Ag/AgCl as a reference electrode, taking a platinum wire as a counter electrode, taking phosphate buffer salt solution as electrolyte, adding DDW solution in which adriamycin ADR is dissolved, measuring electrochemical square wave voltammetry curves under different coexisting concentrations of the ADR by adopting a three-electrode system of an electrochemical workstation, and fitting the oxidation-reduction peak current intensity ratio I of the ADR and Fc ADR /I Fc Constructing a ratio electrochemical sensor based on SNPs@MOF/BNSS-Fc/GCE modified electrode sensing interface with the corresponding ADR coexistence concentration in a linear relation for efficiently detecting the adriamycin ADR, wherein the linear detection range of the ADR concentration is 0.05-5 micromoles/liter, and the detection limit is 0.05 micromolesMol/l.
Example 3
The schematic diagrams of the preparation method and the working principle of the sulfur nanoparticle/MOF/boron nanosheet/ferrocenyl nanosize hybrid ratio electrochemical sensor related to the embodiment are shown in fig. 1, wherein the preparation of sulfur nanoparticle SNPs, SNPs encapsulated in SNPs@MOF hybrids, boron nanosize BNSs and BNSS-Fc complexes is the same as that of embodiment 1, and other specific preparation steps are as follows:
and 5 mu L of 0.5% Nafion ethanol solution is dripped on the surface of a clean glassy carbon electrode GCE, then 5 drops of the BNSS-Fc dispersion liquid are added dropwise, 3 drops of the SNPs@MOF dispersion liquid are added dropwise, one drop of the SNPs@MOF dispersion liquid is dried under a nitrogen flow, and one drop of the SNPs@MOF/BNSS-Fc/GCE modified electrode electrochemical sensing interface is prepared. Inserting the modified electrode serving as a working electrode into an electrolytic tank, taking Ag/AgCl as a reference electrode, taking a platinum wire as a counter electrode, taking phosphate buffer salt solution as electrolyte, adding DDW solution in which adriamycin ADR is dissolved, measuring electrochemical square wave voltammetry curves under different coexisting concentrations of the ADR by adopting a three-electrode system of an electrochemical workstation, and fitting the oxidation-reduction peak current intensity ratio I of the ADR and Fc ADR /I Fc And constructing a ratio electrochemical sensor based on SNPs@MOF/BNSs-Fc/GCE modified electrode sensing interface with the corresponding ADR coexistence concentration in a linear relation, and using the ratio electrochemical sensor to efficiently detect the adriamycin ADR, wherein the linear detection range of the ADR concentration is 0.1-10 micromoles/liter, and the detection limit is 0.1 micromoles/liter.
The foregoing is merely a preferred embodiment of the present invention and it should be noted that modifications and adaptations to those skilled in the art may be made without departing from the principles of the present invention, which are intended to be comprehended within the scope of the present invention.
Claims (1)
1. The preparation method of the sulfur nanoparticle/metal organic framework MOF/boron nanosheet/ferrocenyl nano hybrid ratio electrochemical sensor is characterized by comprising the following steps of:
(1) Dissolving sodium sulfide and sublimed sulfur powder in distilled water DDW, and stirring to obtain polysulfideSodium salt Na 2 S x Adding polyethylene glycol PEG-400 into the solution to form a mixed solution-1; dissolving formic acid and PEG-400 in double distilled water DDW, and uniformly stirring to form a mixed solution-2; dropwise adding the mixed solution-1 into the mixed solution-2, and fully stirring to form a product mixed solution-3; centrifugally separating a product mixed solution-3, washing the obtained precipitate with n-hexane for three times, then washing with ethanol, and carrying out vacuum drying treatment to obtain dried sulfur nanoparticle SNPs powder;
(2) Preparing ethanol solution-1 in which cobalt nitrate hexahydrate is dissolved, and preparing ethanol solution-2 in which 2-methylimidazole is dissolved; adding SNPs powder and polyvinylpyrrolidone PVP into an empty beaker, sequentially adding an ethanol solution-1 and an ethanol solution-2 into the SNPs powder and polyvinylpyrrolidone PVP under sufficient stirring, and performing stirring reaction on the formed mixed solution for a period of time at room temperature; centrifugally separating the product solution after the reaction is finished, washing the product solution for three times by adopting ethanol, and carrying out vacuum drying treatment to obtain SNPs@MOF hybrid powder encapsulated in the dried SNPs, so as to prepare ethanol dispersion;
(3) Preparing a few-layer boron nano-sheets BNSs by adopting an ultrasonic-assisted liquid phase stripping method, preparing ethanol dispersion liquid of the BNSs, then dropwise adding a chloroform solution in which ferrocene Fc is dissolved, and forming ethanol-chloroform dispersion liquid of BNSFc complex under sufficient stirring for standby;
(4) Dropwise adding Nafion solution on the surface of a clean glassy carbon electrode GCE, dropwise adding 1-5 drops of ethanol-chloroform dispersion liquid of BNSS-Fc complex, dropwise adding 1-5 drops of ethanol dispersion liquid of SNPs@MOF hybrid, drying one drop of ethanol dispersion liquid under nitrogen flow after each drop, and finally preparing SNPs@MOF/BNSS-Fc self-assembled nano hybrid modified GCE, wherein the SNPs@MOF/BNSS-Fc self-assembled nano hybrid modified GCE is used as an electrochemical sensing interface;
(5) Inserting SNPs@MOF/BNSs-Fc/GCE serving as a working electrode into an electrolytic cell, taking Ag/AgCl as a reference electrode, taking a platinum wire as a counter electrode, taking phosphate buffer salt solution as electrolyte, adding DDW solution in which adriamycin ADR is dissolved, measuring electrochemical square wave voltammetry curves under different coexisting concentrations of ADR by adopting a three-electrode system of an electrochemical workstation, and fitting the oxidation-reduction peak current intensity ratio I of the ADR and Fc ADR /I Fc Between coexisting concentrations with corresponding ADRAnd (3) constructing a ratio electrochemical sensor based on SNPs@MOF/BNSS-Fc/GCE modified electrode sensing interface in a linear relation, and using the ratio electrochemical sensor to efficiently detect the adriamycin ADR, wherein the linear detection range of the ADR concentration is 0.01-10 micromoles/liter, and the detection limit is 0.01-0.1 micromoles/liter.
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