CN109307673A - A kind of zinc-oxide nano enzyme and its application in preparation quickly detection milk in melamine test paper - Google Patents

A kind of zinc-oxide nano enzyme and its application in preparation quickly detection milk in melamine test paper Download PDF

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Publication number
CN109307673A
CN109307673A CN201811389073.9A CN201811389073A CN109307673A CN 109307673 A CN109307673 A CN 109307673A CN 201811389073 A CN201811389073 A CN 201811389073A CN 109307673 A CN109307673 A CN 109307673A
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China
Prior art keywords
zinc
quantum dot
graphene quantum
oxide nano
modified
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CN201811389073.9A
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Chinese (zh)
Inventor
马振雄
孙鑫
王汉根
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Yangzhou Polytechnic Institute
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Yangzhou Polytechnic Institute
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Priority to CN201811389073.9A priority Critical patent/CN109307673A/en
Publication of CN109307673A publication Critical patent/CN109307673A/en
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    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/75Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated
    • G01N21/77Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator
    • G01N21/78Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator producing a change of colour
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/75Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated
    • G01N21/77Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/75Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated
    • G01N21/77Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator
    • G01N2021/7756Sensor type
    • G01N2021/7759Dipstick; Test strip

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  • Physics & Mathematics (AREA)
  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Plasma & Fusion (AREA)
  • Health & Medical Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Analytical Chemistry (AREA)
  • Biochemistry (AREA)
  • General Health & Medical Sciences (AREA)
  • General Physics & Mathematics (AREA)
  • Immunology (AREA)
  • Pathology (AREA)
  • Measuring Or Testing Involving Enzymes Or Micro-Organisms (AREA)

Abstract

The present invention relates to a kind of zinc-oxide nano enzyme and its applications in preparation quickly detection milk in melamine test paper, the test paper includes blotting paper and reaction film, the reaction film is coated with the detection line of the above-mentioned zinc-oxide nano enzyme based on modified by graphene quantum dot, the material of the reaction film is cellulose membrane, preferably cellulose acetate film, nitrocellulose filter, glass fibre element film or polyester cellulose film.

Description

A kind of zinc-oxide nano enzyme and its melamine test paper in preparation quickly detection milk In application
Technical field
The invention belongs to nano material and melamine detection fields, and in particular to a kind of zinc-oxide nano enzyme and its make Application in standby quickly detection milk in melamine test paper.
Background technique
Melamine (Melamine) is a kind of triazines nitrogen heterocyclic ring organic compound, is slightly soluble in water, be soluble in methanol, The content of glycerol, nitrogen accounts for about 66%, also higher than protein, and cheap, so, some illegal retailers are in order to seek benefit Benefit is added into dairy products or food, causes the illusion of high protein.However, melamine is forbidden adding for food, Long-term intake melamine not only results in reproduction, the damage of urinary system, failure, or even also will cause death.Therefore, accurately The melamine being quickly detected from milk is for guaranteeing that food safety has very important significance.The present invention provides one kind Zinc-oxide nano enzyme based on modified by graphene quantum dot can be used for preparing the test paper of melamine in quickly detection milk.
Summary of the invention
The present invention provides a kind of zinc-oxide nano enzyme based on modified by graphene quantum dot, it is characterised in that described to be based on stone The preparation method of the zinc-oxide nano enzyme of black alkene quantum dot modification includes the following steps:
Graphene quantum dot solution is added into zinc nitrate solution, after stirring 10min, it is molten that alkali metal hydroxide is added Liquid continues after stirring 10min, is warming up to 140 DEG C, reacts 12 hours, cooled to room temperature, filtering, precipitating deionized water, After ethanol washing, 10h is dried in vacuo at 80 DEG C to get the zinc-oxide nano enzyme based on modified by graphene quantum dot.
The concentration of the zinc nitrate solution is 0.1mol/L, and the concentration of graphene quantum dot solution is 1.0mg/mL, alkali gold The concentration for belonging to hydroxide solution is 0.1mol/L, and every mM of zinc nitrate uses graphene quantum dot solution 5mL, uses alkali gold Belong to hydroxide solution 10mL.
The preferred sodium hydroxide of the alkali metal hydroxide or potassium hydroxide.It is described reaction preferably in a high pressure reaction kettle into Row.
Another embodiment of the present invention provides the above-mentioned zinc-oxide nano enzyme based on modified by graphene quantum dot and is detecting Application in melamine.Especially in the application of detection melamine in dairy products.
Another embodiment of the present invention provides the above-mentioned zinc-oxide nano enzyme based on modified by graphene quantum dot and is preparing Quickly detect the application of melamine test paper in milk.
Another embodiment of the present invention provides one kind and quickly detects melamine test paper in milk, it is characterised in that described Test paper includes blotting paper and reaction film, and the reaction film is coated with the above-mentioned zinc-oxide nano enzyme based on modified by graphene quantum dot Detection line, the material of the reaction film is cellulose membrane, preferably cellulose acetate film, nitrocellulose filter, glass fibre element Film or polyester cellulose film.
The blotting paper is blotting paper commonly used in the art, thickness 0.3-0.5mm, rate of water absorption 5-10s/4cm, water absorption 300-500mg/cm2
Compared with the prior art, the advantages of the present invention are as follows: the present invention is based on modified by graphene quantum dot to obtain zinc oxide Nano enzyme, the test paper of preparation can be used for directly quickly detecting the middle melamine of the dairy products such as milk, and detection limit reaches 25ppm.
Detailed description of the invention
Fig. 1 is the SEM figure of product A.
Specific embodiment
For the ease of a further understanding of the present invention, examples provided below has done more detailed description to it.But It is that these embodiments are only not supposed to be a limitation to the present invention or implementation principle for better understanding invention, reality of the invention The mode of applying is not limited to the following contents.
Embodiment 1
Graphene quantum dot solution (1.0mg/mL, 5mL) is added in zinc nitrate solution (0.1mol/L, 10mL), stirring It after 10min, is added sodium hydroxide solution (0.1mol/L, 10mL), continues after stirring 10min, be warming up to 140 DEG C, reaction 12 is small When, cooled to room temperature, filtering is precipitated with after deionized water, ethanol washing, and vacuum drying 10h is at 80 DEG C to get described Zinc-oxide nano enzyme (78mg, hereinafter referred to as product A) based on modified by graphene quantum dot.
Embodiment 2
Graphene quantum dot solution (1.0mg/mL, 5mL) is added in zinc nitrate solution (0.1mol/L, 10mL), stirring It after 10min, is added potassium hydroxide solution (0.1mol/L, 10mL), continues after stirring 10min, be warming up to 140 DEG C, reaction 12 is small When, cooled to room temperature, filtering is precipitated with after deionized water, ethanol washing, and vacuum drying 10h is at 80 DEG C to get described Zinc-oxide nano enzyme based on modified by graphene quantum dot (pattern is consistent with product A under scanning electron microscope).
Embodiment 3
Firstly, product A is sprayed on reaction film (nitrocellulose filter or polyester cellulose film) using film metal spraying mark machine is drawn On detection line is made;Then reaction film and blotting paper are pasted, the test strips for needing specification are cut into dedicated cutting machine, (such as 4.0 × 55mm).The blotting paper is blotting paper commonly used in the art, thickness 0.3-0.5mm, rate of water absorption 5-10s/ 4cm, water absorption 300-500mg/cm2
Embodiment 4
Fresh milk is taken, appropriate melamine is added, is configured to the sample to be tested that content of melamine is 200mg/L, then Dilution is made into the sample to be tested that concentration is 100,50,25,12.5,6.25mg/L respectively.
The sample to be tested of various concentration and fresh milk (blank control) are added drop-wise to the test strips of the preparation of embodiment 3 respectively On, observed after 30s, be added dropwise concentration be 200,100,50, occur clearly at the test strips detection line of 25mg/L sample to be tested Blue detection line, only dropwise addition fresh milk (blank control) and concentration are the test strips detection of 12.5,6.25mg/L sample to be tested Do not occur blue detection line at line.Be repeated 5 times test, be added dropwise concentration be 200,100,50,25,6.25mg/L sample to be tested and fresh The testing result of the test strips of milk (blank control) is consistent;Wherein having 3 tests that concentration is added dropwise is 12.5mg/L sample to be tested Indistinctly there is detection line at the detection line of test strips.The result shows that test strips of the present invention detect the detection of melamine in milk It is limited to 25mg/L (being equivalent to 25ppm).

Claims (10)

1. a kind of zinc-oxide nano enzyme based on modified by graphene quantum dot, it is characterised in that described to be repaired based on graphene quantum dot The preparation method of the zinc-oxide nano enzyme of decorations includes the following steps:
Graphene quantum dot solution is added into zinc nitrate solution, after stirring 10min, alkali hydroxide soln is added, after After continuous stirring 10min, 140 DEG C are warming up to, is reacted 12 hours, cooled to room temperature, filtering, precipitating deionized water, ethyl alcohol After washing, 10h is dried in vacuo at 80 DEG C to get the zinc-oxide nano enzyme based on modified by graphene quantum dot.
2. the zinc-oxide nano enzyme described in claim 1 based on modified by graphene quantum dot, it is characterised in that the zinc nitrate The concentration of solution is 0.1mol/L, and the concentration of graphene quantum dot solution is 1.0mg/mL, alkali hydroxide soln it is dense Degree is 0.1mol/L, and every mM of zinc nitrate uses graphene quantum dot solution 5mL, uses alkali hydroxide soln 10mL。
3. the described in any item zinc-oxide nano enzymes based on modified by graphene quantum dot of claim 1-2, it is characterised in that institute State the preferred sodium hydroxide of alkali metal hydroxide or potassium hydroxide.
4. the described in any item zinc-oxide nano enzymes based on modified by graphene quantum dot of claim 1-3 are in detection melamine In application.
5. application as claimed in claim 4, it is characterised in that the application in detection melamine in dairy products.
6. the described in any item zinc-oxide nano enzymes based on modified by graphene quantum dot of claim 1-3 are in preparation quickly detection Application in milk in melamine test paper.
7. the test paper of melamine in a kind of quickly detection milk, it is characterised in that the test paper includes blotting paper and reaction film, The reaction film is coated with the detection line of the above-mentioned zinc-oxide nano enzyme based on modified by graphene quantum dot.
8. test paper as claimed in claim 7, it is characterised in that the material of the reaction film is cellulose membrane, preferably cellulose acetate Film, nitrocellulose filter, glass fibre element film or polyester cellulose film.
9. the described in any item test paper of claim 7-8, it is characterised in that the blotting paper is blotting paper commonly used in the art, thick Spend 0.3-0.5mm, rate of water absorption 5-10s/4cm, water absorption 300-500mg/cm2
10. the preparation method of the described in any item zinc-oxide nano enzymes based on modified by graphene quantum dot of claim 1-3.
CN201811389073.9A 2018-11-20 2018-11-20 A kind of zinc-oxide nano enzyme and its application in preparation quickly detection milk in melamine test paper Pending CN109307673A (en)

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Citations (5)

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Publication number Priority date Publication date Assignee Title
CN102156118A (en) * 2011-03-22 2011-08-17 中国科学院长春应用化学研究所 Method for detecting melamine
US20120140216A1 (en) * 2010-12-07 2012-06-07 Sony Corporation Method for evaluation of oxide semiconductor electrode, apparatus for evaluation of oxide semiconductor electrode, and apparatus for production of oxide semiconductor electrode
CN104098088A (en) * 2014-06-17 2014-10-15 华南理工大学 Preparation method for nano-zinc oxide modified graphene hybrid material
CN104941643A (en) * 2015-06-16 2015-09-30 北京科技大学 Preparation method of Ag-GQDs(Graphene Quantum Dots)/ZnO ternary photocatalyst
CN107321375A (en) * 2017-07-13 2017-11-07 扬州工业职业技术学院 A kind of SiO2/ZnO/g‑C3N4Nano material and its application in reduction of hexavalent chromium

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20120140216A1 (en) * 2010-12-07 2012-06-07 Sony Corporation Method for evaluation of oxide semiconductor electrode, apparatus for evaluation of oxide semiconductor electrode, and apparatus for production of oxide semiconductor electrode
CN102156118A (en) * 2011-03-22 2011-08-17 中国科学院长春应用化学研究所 Method for detecting melamine
CN104098088A (en) * 2014-06-17 2014-10-15 华南理工大学 Preparation method for nano-zinc oxide modified graphene hybrid material
CN104941643A (en) * 2015-06-16 2015-09-30 北京科技大学 Preparation method of Ag-GQDs(Graphene Quantum Dots)/ZnO ternary photocatalyst
CN107321375A (en) * 2017-07-13 2017-11-07 扬州工业职业技术学院 A kind of SiO2/ZnO/g‑C3N4Nano material and its application in reduction of hexavalent chromium

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Title
XIANGFENG CHU ET AL.: "The acetic acid gas sensing properties of graphene quantum dots (GQDs)–ZnO nanocomposites prepared by hydrothermal method", 《J MATER SCI: MATER ELECTRON》 *
YING LI ET AL.: "Chemical sensors and biosensors for the detection of melamine", 《RSC ADVANCES》 *
吴世敏 等: "《简明精细化工大辞典》", 30 June 1996, 辽宁科学技术出版社 *
张俊: "石墨烯(量子点)—锌锡氧化物复合材料气敏性能研究", 《中国优秀硕士论文全文数据库 工程科技I辑》 *
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