CN103961343A - Preparation method of L-cysteine- graphene oxide nano material - Google Patents

Preparation method of L-cysteine- graphene oxide nano material Download PDF

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CN103961343A
CN103961343A CN201410170050.4A CN201410170050A CN103961343A CN 103961343 A CN103961343 A CN 103961343A CN 201410170050 A CN201410170050 A CN 201410170050A CN 103961343 A CN103961343 A CN 103961343A
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cys
nano material
graphene oxide
graphene
preparation
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CN103961343B (en
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胡献刚
刘琦
周启星
陈玉明
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Nankai University
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Nankai University
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Abstract

The invention provides a preparation method of L-cysteine-graphene oxide nano material. The preparation method comprises the following steps: (1) adding graphene oxide to purified water to obtain graphene oxide suspension; (2) adding 1-(3-dimethylaminopropyl)-3-ethylcarbodiimide hydrochloride and N-hydroxysulfosuccinimide sodium salt to obtain a mixed solution, and conducting an activating reaction for 1 h; (3) adding L-cysteine for reaction for 12 h; filtering through a 0.22-micron ultrafiltration membrane; freeze-drying the solid at 50 DEG C below zero. The prepared L-cysteine-graphene oxide nano material can be used for reducing toxicity in a zebrafish embryo exposed to arsenic. The preparation method has the advantages that the process is simple and is easy to carry out; the L-cysteine-graphene oxide nano material can reduce the aberration rate of the zebrafish embryo by 15% when used in a test for reducing the toxicity in the zebrafish embryo exposed to the arsenic.

Description

A kind of preparation method of Cys-stannic oxide/graphene nano material
Technical field
The present invention relates to reduce preparation and the application of arsenic toxicity nano material, concrete is a kind of preparation method of Cys-stannic oxide/graphene nano material.
Background technology
The character such as that the compound of arsenic has is carcinogenic, teratogenesis, mutagenesis.Arseniasis is taking skin as main systemic disease, skin that it can harmful to human, breathing, digestion, urinary system, cardiovascular, nerve, hemopoietic system etc.The exploitation of arsenic polluted underground water, cause China's water to occur that serious arsenic pollutes, and has had a strong impact on health containing use, the metal smelt etc. of arsenic agriculture chemical.
Water-soluble nano graphene oxide be a kind of surface with oxy radical and be nano material, can, under oxidation and ultrasonic condition, utilize block graphite to make, with low cost.After further chemical modification, can under physiological condition, keep good stability and not reunite.The Cys that it can load alleviates arsenic toxicity, makes it can enter better receptor biological, alleviates arsenic toxicity.
Biological subject used in the present invention is zebrafish embryo.Zebrafish embryo external fertilization, ectogenesis, idiosome are transparent, can be observed all internals and structure and growth course thereof from complete live body, also observe the indicator reaction of nearly 20 kinds of different manifestations, can this judge the mechanism of toxication of pollutant.And Brachydanio rerio, there is the similarity of height aspect heredity, physiology and pharmacological reaction with the mankind, therefore can be used as good model animal.
Summary of the invention
The object of the invention is for above-mentioned existing problems, a kind of preparation method and application of Cys-stannic oxide/graphene nano material are provided, this preparation method technique is simple, easy to implement, dyes arsenic toxicity test for zebrafish embryo, can make the abnormal rate of zebrafish embryo reduce by 15%.
Technical scheme of the present invention:
A kind of preparation method of Cys-stannic oxide/graphene nano material, step is as follows:
1) graphene oxide is added to ultrasonic agitation 1h in pure water, obtain the graphene oxide suspension of relative homogeneous;
2) in above-mentioned graphene oxide suspension, adding 1-(3-dimethylaminopropyl)-3-ethyl-carbodiimide hydrochloride and N-hydroxy-succinamide sulfonate sodium obtain mixed liquor, under stirring condition, graphene oxide surface carboxyl is carried out to priming reaction, the priming reaction time is 1h;
3) will in the mixed liquor after above-mentioned priming reaction, add Cys, react 12h, then use the ultrafiltration membrance filter of 0.22um, by the lyophilization at-50 DEG C of gained solids, can make Cys-stannic oxide/graphene nano material.
The concentration of described graphene oxide suspension is 8mg/mL.
Graphene oxide, 1-(3-dimethylaminopropyl in described mixed liquor) amount ratio of-3-ethyl-carbodiimide hydrochloride and N-hydroxy-succinamide sulfonate sodium is 10mL:0.2M:0.5M.
In mixed liquor after described priming reaction, graphene oxide and Cys mass ratio are 1:0.1-10.
An application for prepared Cys-stannic oxide/graphene nano material, dyes arsenic toxicity for reducing zebrafish embryo.
Advantage of the present invention is: the preparation method technique of this Cys-stannic oxide/graphene nano material is simple, easy to implement, dyes arsenic toxicity test for reducing zebrafish embryo, can make the abnormal rate of zebrafish embryo reduce by 15%.
Brief description of the drawings
Fig. 1 is that after adding natrium arsenicum contamination, pericardium edema figure appearred in zebrafish embryo at the 5th day.
Fig. 2 is that after adding natrium arsenicum contamination, rachiocamposis figure appearred in zebrafish embryo at the 5th day.
Fig. 3 adds zebrafish embryo after nano material of the present invention at the aspect graph of the 5th day.
Detailed description of the invention
Embodiment 1:
A kind of preparation method of Cys-stannic oxide/graphene nano material, step is as follows:
1) graphene oxide is added to ultrasonic agitation 1h in pure water, obtain the graphene oxide suspension of relative homogeneous, the concentration of graphene oxide suspension is 8mg/mL;
2) in above-mentioned 10mL graphene oxide suspension, adding the 1-(3-dimethylaminopropyl of 0.2M) the N-hydroxy-succinamide sulfonate sodium of-3-ethyl-carbodiimide hydrochloride and 0.5M obtains mixed liquor, under stirring condition, graphene oxide surface carboxyl is carried out to priming reaction, the priming reaction time is 1h;
3) Cys of 8mg will be added in the mixed liquor after above-mentioned priming reaction, making graphene oxide and Cys mass ratio is 1:0.1, reaction 12h, then use the ultrafiltration membrance filter of 0.22um, by the lyophilization at-50 DEG C of gained solids, can make Cys-stannic oxide/graphene nano material.
By Cys-stannic oxide/graphene nano material of preparation for reducing zebrafish embryo dye arsenic toxicity, experimental technique is as follows:
First prepare embryo medium, described embryo medium is E3 culture fluid, and in every 1000L deionized water, containing 292.5g sodium chloride, 12.67g potassium chloride, 36.63g calcium chloride and 39.6g magnesium sulfate, regulating pH value with sodium bicarbonate solution is 7.2, electrical conductivity 600uS.
With above-mentioned embryo medium, the Cys-stannic oxide/graphene nano material making is made into the solution of 1mg/L, cultivate the embryo through the natrium arsenicum contamination of 1mg/L, at 120 hours observation Brachydanio rerio abnormal rates, its abnormal rate was than directly having reduced 10-15% with the embryo of natrium arsenicum contamination.
Fig. 1 is that after adding natrium arsenicum contamination, pericardium edema figure appearred in zebrafish embryo at the 5th day; Fig. 2 is that after adding natrium arsenicum contamination, rachiocamposis figure appearred in zebrafish embryo at the 5th day.
Fig. 3 adds zebrafish embryo after nano material of the present invention at the aspect graph of the 5th day, shows: Brachydanio rerio has grown normal organ and tissue in figure, does not occur lopsided situation.
Embodiment 2:
A kind of preparation method of Cys-stannic oxide/graphene nano material, step is as follows:
1) graphene oxide is added to ultrasonic agitation 1h in pure water, obtain the graphene oxide suspension of relative homogeneous, the concentration of graphene oxide suspension is 8mg/mL;
2) in above-mentioned 10mL graphene oxide suspension, adding the 1-(3-dimethylaminopropyl of 0.2M) the N-hydroxy-succinamide sulfonate sodium of-3-ethyl-carbodiimide hydrochloride and 0.5M obtains mixed liquor, under stirring condition, graphene oxide surface carboxyl is carried out to priming reaction, the priming reaction time is 1h;
3) Cys of 80mg will be added in the mixed liquor after above-mentioned priming reaction, making graphene oxide and Cys mass ratio is 1:0.1, reaction 12h, then use the ultrafiltration membrance filter of 0.22um, by the lyophilization at-50 DEG C of gained solids, can make Cys-stannic oxide/graphene nano material.
By Cys-stannic oxide/graphene nano material of preparation for reducing zebrafish embryo dye arsenic toxicity, experimental technique is as follows:
The preparation method of embryo medium is identical with embodiment 1.
With embryo medium, the Cys-stannic oxide/graphene nano material making is made into the solution of 1mg/L, cultivate the embryo through the natrium arsenicum contamination of 1mg/L, at 120 hours observation Brachydanio rerio abnormal rates, its abnormal rate was than directly having reduced 10-15% with the embryo of natrium arsenicum contamination.
Embodiment 3:
A kind of preparation method of Cys-stannic oxide/graphene nano material, step is as follows:
1) graphene oxide is added to ultrasonic agitation 1h in pure water, obtain the graphene oxide suspension of relative homogeneous, the concentration of graphene oxide suspension is 8mg/mL;
2) in above-mentioned 10mL graphene oxide suspension, adding the 1-(3-dimethylaminopropyl of 0.2M) the N-hydroxy-succinamide sulfonate sodium of-3-ethyl-carbodiimide hydrochloride and 0.5M obtains mixed liquor, under stirring condition, graphene oxide surface carboxyl is carried out to priming reaction, the priming reaction time is 1h;
3) Cys of 800mg will be added in the mixed liquor after above-mentioned priming reaction, making graphene oxide and Cys mass ratio is 1:0.1, reaction 12h, then use the ultrafiltration membrance filter of 0.22um, by the lyophilization at-50 DEG C of gained solids, can make Cys-stannic oxide/graphene nano material.
By Cys-stannic oxide/graphene nano material of preparation for reducing zebrafish embryo dye arsenic toxicity, experimental technique is as follows:
The preparation method of embryo medium is identical with embodiment 1.
With embryo medium, the Cys-stannic oxide/graphene nano material making is made into the solution of 1mg/L, cultivate the embryo through the natrium arsenicum contamination of 1mg/L, at 120 hours observation Brachydanio rerio abnormal rates, its abnormal rate was than directly having reduced 10-15% with the embryo of natrium arsenicum contamination.

Claims (5)

1. a preparation method for Cys-stannic oxide/graphene nano material, is characterized in that step is as follows:
1) graphene oxide is added to ultrasonic agitation 1h in pure water, obtain the graphene oxide suspension of relative homogeneous;
2) in above-mentioned graphene oxide suspension, adding 1-(3-dimethylaminopropyl)-3-ethyl-carbodiimide hydrochloride and N-hydroxy-succinamide sulfonate sodium obtain mixed liquor, under stirring condition, graphene oxide surface carboxyl is carried out to priming reaction, the priming reaction time is 1h;
3) will in the mixed liquor after above-mentioned priming reaction, add Cys, react 12h, then use the ultrafiltration membrance filter of 0.22um, by the lyophilization at-50 DEG C of gained solids, can make Cys-stannic oxide/graphene nano material.
2. the preparation method of Cys-stannic oxide/graphene nano material according to claim 1, is characterized in that: the concentration of described graphene oxide suspension is 8mg/mL.
3. the preparation method of Cys-stannic oxide/graphene nano material according to claim 1, is characterized in that: graphene oxide, 1-(3-dimethylaminopropyl in described mixed liquor) amount ratio of-3-ethyl-carbodiimide hydrochloride and N-hydroxy-succinamide sulfonate sodium is 10mL:0.2M:0.5M.
4. the preparation method of Cys-stannic oxide/graphene nano material according to claim 1, is characterized in that: in the mixed liquor after described priming reaction, graphene oxide and Cys mass ratio are 1:0.1-10.
5. an application for Cys-stannic oxide/graphene nano material as prepared in claim 1, is characterized in that: dye arsenic toxicity for reducing zebrafish embryo.
CN201410170050.4A 2014-04-25 2014-04-25 A kind of preparation method of Cys-stannic oxide/graphene nano material Expired - Fee Related CN103961343B (en)

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106496585A (en) * 2016-10-21 2017-03-15 浙江大学 Sensitive graphene oxide based nano-materials of a kind of ROS and its preparation method and application
CN107936035A (en) * 2017-11-29 2018-04-20 温州医科大学 A kind of cysteine-modifying graphene quantum dot GQCY and preparation method are with preparing the application on dopamine luciferase assay reagent
CN109896638A (en) * 2019-03-22 2019-06-18 湖州师范学院 Application of the degradation of microcystins enzyme in degradation nodularins

Non-Patent Citations (3)

* Cited by examiner, † Cited by third party
Title
OMID AKHAVAN ET AL: "Genotoxicity of graphene nanoribbons in human mesenchymal stem cells", 《CARBON》, 7 December 2012 (2012-12-07), pages 419 - 431 *
XIANGANG HU ET AL: "Covalently synthesized graphene oxide-aptamer nanosheets for efficient visible-light photocatalysis of nucleic acids and proteins of viruses", 《CARBON》, 22 February 2012 (2012-02-22), pages 2772 - 2781 *
XIAO ZHI ET AL: "The immunotoxicity of graphene oxides and the effect of PVP-coating", 《BIOMATERIALS》, vol. 34, 6 April 2013 (2013-04-06), pages 5254 - 5261, XP028593822, DOI: doi:10.1016/j.biomaterials.2013.03.024 *

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106496585A (en) * 2016-10-21 2017-03-15 浙江大学 Sensitive graphene oxide based nano-materials of a kind of ROS and its preparation method and application
CN106496585B (en) * 2016-10-21 2019-02-19 浙江大学 A kind of graphene oxide based nano-material and its preparation method and application of ROS sensitivity
CN107936035A (en) * 2017-11-29 2018-04-20 温州医科大学 A kind of cysteine-modifying graphene quantum dot GQCY and preparation method are with preparing the application on dopamine luciferase assay reagent
CN109896638A (en) * 2019-03-22 2019-06-18 湖州师范学院 Application of the degradation of microcystins enzyme in degradation nodularins
CN109896638B (en) * 2019-03-22 2021-11-02 湖州师范学院 Application of microcystin degrading enzyme in degradation of nodulococcus toxin

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