Method Article
Protocol for the synthesis of Cys-nFeS
Lizeng Gao
Gao Lab (Yangzhou University)
Corresponding Author
Abstract
To produce our target nanozyme with a narrow size distribution, solvothermal method was performed to composite iron sulfide at high temperatures and pressures. Here we describe the protocol for synthesizing Cys-nFeS.
Keywords
Iron oxide, nanoparticles, cysteine, solvothermal
Figures
Figure 1
Introduction
To produce inorganic polysulfide from organosulfur compound, solvothermal method was performed to prepare nano-iron sulfide at high temperature and pressure in a sealed autoclave reactor1,2. Here we describe the protocol for synthesizing Cys-nFeS.
Reagents
ethylene glycol, FeCl3•6H2O, Sodium acetate(NaOAc), cysteine
Equipment
magnetic stirring bar, oven, Teflon-lined stainless steel autoclave
Procedure
- 0.82 g FeCl3•6H2O was dissolved uniformly in 40 mL ethylene glycol in a beaker.
- Keep stirring the mixture with a stir bar till it turned orange without distinct precipitation. CAUTION If the reactants added into the ethylene glycol cannot be dispersed easily, ultrasonic treatment on the mixture for 10 min or even longer would help.
- 3.6 g Sodium acetate was added into the mixture until the iron source was totally dissolved and the suspension became dark brown.
- Appropriate amount of cysteine were added into the mixture during the mixing process respectively.
- The mixture was transferred into a 50 mL Teflon-lined stainless steel autoclave in the fume cupboard after being sufficiently stirred and sonicated. CAUTION The screws of the stainless steel autoclave should be tightened for guaranteed pressure and safety.
- The reaction was conducted at 200℃ in an oven for 12 h.
- After the reaction was finished, the Teflon-lined stainless steel autoclave was cooled to room temperature.
- The products in the Teflon-lined stainless steel autoclave was poured into a 50 mL centrifuge tube with the supernatant discarded.
- The products was dissolved in ethanol and washed for several times through centrifugal separation at 5000 g for 5 min until the washings became clear.
- The product of Cys-nFeS was obtained after drying at 60℃ for 4 h, and then preserved at 4℃
Timing
14 h or longer(including the mixing process and the reaction time under high temperature and high pressure)
Anticipated Results
The new formed products are black powder which consist of hexagonal sheet-like nanostructures and sphere nanoparticles characterized by electron microscope.
References
1.Gao, L. et al. Intrinsic peroxidase-like activity of ferromagnetic nanoparticles. Nat Nanotechnol 2, 577-583(2007).
2.Gao, L. Z. et al. Magnetite Nanoparticle-Linked Immunosorbent Assay. J Phys Chem C 112, 17357-17361(2008).
3.Fan, K. et al. Optimization of Fe3O4 nanozyme activity via single amino acid modification mimicking an enzyme active site.Chem Commun 53, 424-427(2016).
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Posted 03 Dec, 2018
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Subject Areas
Nanoscience and technology
Associated Publications
Converting organosulfur compounds to inorganic polysulfides against resistant bacterial infections
by Zhuobin Xu, Zhiyue Qiu, Qi Liu, +15
Nature Communications (22 November, 2018)
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Method Article
Protocol for the synthesis of Cys-nFeS
Lizeng Gao
Gao Lab (Yangzhou University)
Corresponding Author
Article
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Abstract
To produce our target nanozyme with a narrow size distribution, solvothermal method was performed to composite iron sulfide at high temperatures and pressures. Here we describe the protocol for synthesizing Cys-nFeS.
Figures
Figure 1
Introduction
To produce inorganic polysulfide from organosulfur compound, solvothermal method was performed to prepare nano-iron sulfide at high temperature and pressure in a sealed autoclave reactor1,2. Here we describe the protocol for synthesizing Cys-nFeS.
Reagents
ethylene glycol, FeCl3•6H2O, Sodium acetate(NaOAc), cysteine
Equipment
magnetic stirring bar, oven, Teflon-lined stainless steel autoclave
Procedure
- 0.82 g FeCl3•6H2O was dissolved uniformly in 40 mL ethylene glycol in a beaker.
- Keep stirring the mixture with a stir bar till it turned orange without distinct precipitation. CAUTION If the reactants added into the ethylene glycol cannot be dispersed easily, ultrasonic treatment on the mixture for 10 min or even longer would help.
- 3.6 g Sodium acetate was added into the mixture until the iron source was totally dissolved and the suspension became dark brown.
- Appropriate amount of cysteine were added into the mixture during the mixing process respectively.
- The mixture was transferred into a 50 mL Teflon-lined stainless steel autoclave in the fume cupboard after being sufficiently stirred and sonicated. CAUTION The screws of the stainless steel autoclave should be tightened for guaranteed pressure and safety.
- The reaction was conducted at 200℃ in an oven for 12 h.
- After the reaction was finished, the Teflon-lined stainless steel autoclave was cooled to room temperature.
- The products in the Teflon-lined stainless steel autoclave was poured into a 50 mL centrifuge tube with the supernatant discarded.
- The products was dissolved in ethanol and washed for several times through centrifugal separation at 5000 g for 5 min until the washings became clear.
- The product of Cys-nFeS was obtained after drying at 60℃ for 4 h, and then preserved at 4℃
Timing
14 h or longer(including the mixing process and the reaction time under high temperature and high pressure)
Anticipated Results
The new formed products are black powder which consist of hexagonal sheet-like nanostructures and sphere nanoparticles characterized by electron microscope.
References
1.Gao, L. et al. Intrinsic peroxidase-like activity of ferromagnetic nanoparticles. Nat Nanotechnol 2, 577-583(2007).
2.Gao, L. Z. et al. Magnetite Nanoparticle-Linked Immunosorbent Assay. J Phys Chem C 112, 17357-17361(2008).
3.Fan, K. et al. Optimization of Fe3O4 nanozyme activity via single amino acid modification mimicking an enzyme active site.Chem Commun 53, 424-427(2016).
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