CN106841186B - A kind of method of quick detection pymetrozine - Google Patents
A kind of method of quick detection pymetrozine Download PDFInfo
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- CN106841186B CN106841186B CN201710075857.3A CN201710075857A CN106841186B CN 106841186 B CN106841186 B CN 106841186B CN 201710075857 A CN201710075857 A CN 201710075857A CN 106841186 B CN106841186 B CN 106841186B
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- 239000005925 Pymetrozine Substances 0.000 title claims abstract description 107
- QHMTXANCGGJZRX-WUXMJOGZSA-N pymetrozine Chemical compound C1C(C)=NNC(=O)N1\N=C\C1=CC=CN=C1 QHMTXANCGGJZRX-WUXMJOGZSA-N 0.000 title claims abstract description 107
- 238000001514 detection method Methods 0.000 title claims abstract description 63
- 238000000034 method Methods 0.000 title claims abstract description 27
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 claims abstract description 75
- 239000010931 gold Substances 0.000 claims abstract description 75
- 229910052737 gold Inorganic materials 0.000 claims abstract description 75
- 239000002105 nanoparticle Substances 0.000 claims abstract description 69
- 229920000877 Melamine resin Polymers 0.000 claims abstract description 57
- JDSHMPZPIAZGSV-UHFFFAOYSA-N melamine Chemical group NC1=NC(N)=NC(N)=N1 JDSHMPZPIAZGSV-UHFFFAOYSA-N 0.000 claims abstract description 50
- 230000008859 change Effects 0.000 claims abstract description 49
- 238000010521 absorption reaction Methods 0.000 claims abstract description 33
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 26
- 239000001257 hydrogen Substances 0.000 claims abstract description 4
- 229910052739 hydrogen Inorganic materials 0.000 claims abstract description 4
- 239000000243 solution Substances 0.000 claims description 158
- 239000007864 aqueous solution Substances 0.000 claims description 63
- 239000001509 sodium citrate Substances 0.000 claims description 31
- NLJMYIDDQXHKNR-UHFFFAOYSA-K sodium citrate Chemical compound O.O.[Na+].[Na+].[Na+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O NLJMYIDDQXHKNR-UHFFFAOYSA-K 0.000 claims description 31
- 230000004048 modification Effects 0.000 claims description 29
- 238000012986 modification Methods 0.000 claims description 29
- 239000007788 liquid Substances 0.000 claims description 24
- 230000000052 comparative effect Effects 0.000 claims description 20
- 244000269722 Thea sinensis Species 0.000 claims description 14
- 235000009569 green tea Nutrition 0.000 claims description 14
- 235000019987 cider Nutrition 0.000 claims description 12
- 238000003756 stirring Methods 0.000 claims description 11
- 238000007306 functionalization reaction Methods 0.000 claims description 10
- 239000001508 potassium citrate Substances 0.000 claims description 7
- 229960002635 potassium citrate Drugs 0.000 claims description 7
- QEEAPRPFLLJWCF-UHFFFAOYSA-K potassium citrate (anhydrous) Chemical compound [K+].[K+].[K+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O QEEAPRPFLLJWCF-UHFFFAOYSA-K 0.000 claims description 7
- 235000011082 potassium citrates Nutrition 0.000 claims description 7
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims description 5
- 238000009835 boiling Methods 0.000 claims description 5
- 238000006243 chemical reaction Methods 0.000 claims description 5
- 239000011734 sodium Substances 0.000 claims description 5
- 229910052708 sodium Inorganic materials 0.000 claims description 5
- 238000007689 inspection Methods 0.000 claims description 4
- 230000035484 reaction time Effects 0.000 claims description 4
- 239000012488 sample solution Substances 0.000 claims description 4
- 239000003638 chemical reducing agent Substances 0.000 claims description 3
- XZMCDFZZKTWFGF-UHFFFAOYSA-N Cyanamide Chemical compound NC#N XZMCDFZZKTWFGF-UHFFFAOYSA-N 0.000 claims 2
- KAESVJOAVNADME-UHFFFAOYSA-N Pyrrole Chemical compound C=1C=CNC=1 KAESVJOAVNADME-UHFFFAOYSA-N 0.000 claims 2
- 238000005829 trimerization reaction Methods 0.000 claims 2
- 241001124076 Aphididae Species 0.000 claims 1
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical group [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 claims 1
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 claims 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims 1
- 239000011260 aqueous acid Substances 0.000 claims 1
- 229910052796 boron Inorganic materials 0.000 claims 1
- 239000000460 chlorine Substances 0.000 claims 1
- 229910052801 chlorine Inorganic materials 0.000 claims 1
- 150000002576 ketones Chemical class 0.000 claims 1
- 230000009471 action Effects 0.000 abstract description 3
- 230000035945 sensitivity Effects 0.000 abstract description 3
- 239000002086 nanomaterial Substances 0.000 abstract 1
- 230000009467 reduction Effects 0.000 description 39
- 238000002360 preparation method Methods 0.000 description 15
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 12
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 description 12
- 229920000642 polymer Polymers 0.000 description 8
- 235000013339 cereals Nutrition 0.000 description 7
- 150000007974 melamines Chemical class 0.000 description 7
- 239000012279 sodium borohydride Substances 0.000 description 6
- 229910000033 sodium borohydride Inorganic materials 0.000 description 6
- 238000013019 agitation Methods 0.000 description 5
- 239000002917 insecticide Substances 0.000 description 5
- 235000013305 food Nutrition 0.000 description 4
- 238000010438 heat treatment Methods 0.000 description 4
- 238000000862 absorption spectrum Methods 0.000 description 3
- 230000008569 process Effects 0.000 description 3
- 229910003803 Gold(III) chloride Inorganic materials 0.000 description 2
- 240000007594 Oryza sativa Species 0.000 description 2
- 235000007164 Oryza sativa Nutrition 0.000 description 2
- 241000607479 Yersinia pestis Species 0.000 description 2
- 235000015203 fruit juice Nutrition 0.000 description 2
- 235000011389 fruit/vegetable juice Nutrition 0.000 description 2
- JMANVNJQNLATNU-UHFFFAOYSA-N glycolonitrile Natural products N#CC#N JMANVNJQNLATNU-UHFFFAOYSA-N 0.000 description 2
- RJHLTVSLYWWTEF-UHFFFAOYSA-K gold trichloride Chemical compound Cl[Au](Cl)Cl RJHLTVSLYWWTEF-UHFFFAOYSA-K 0.000 description 2
- 238000004128 high performance liquid chromatography Methods 0.000 description 2
- 230000007246 mechanism Effects 0.000 description 2
- 239000012528 membrane Substances 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 235000009566 rice Nutrition 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- QMNWYGTWTXOQTP-UHFFFAOYSA-N 1h-triazin-6-one Chemical compound O=C1C=CN=NN1 QMNWYGTWTXOQTP-UHFFFAOYSA-N 0.000 description 1
- 206010019233 Headaches Diseases 0.000 description 1
- 206010020772 Hypertension Diseases 0.000 description 1
- 241000251539 Vertebrata <Metazoa> Species 0.000 description 1
- 206010047700 Vomiting Diseases 0.000 description 1
- DOXNPNNLGSPXBC-UHFFFAOYSA-N [Au].NC1=NC(N)=NC(N)=N1 Chemical compound [Au].NC1=NC(N)=NC(N)=N1 DOXNPNNLGSPXBC-UHFFFAOYSA-N 0.000 description 1
- 150000001412 amines Chemical class 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 230000000711 cancerogenic effect Effects 0.000 description 1
- 231100000357 carcinogen Toxicity 0.000 description 1
- 239000003183 carcinogenic agent Substances 0.000 description 1
- 238000005119 centrifugation Methods 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000001736 differential pulse polarography Methods 0.000 description 1
- 201000010099 disease Diseases 0.000 description 1
- 208000037265 diseases, disorders, signs and symptoms Diseases 0.000 description 1
- 235000013399 edible fruits Nutrition 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 235000021393 food security Nutrition 0.000 description 1
- 238000004817 gas chromatography Methods 0.000 description 1
- 150000002343 gold Chemical class 0.000 description 1
- FDWREHZXQUYJFJ-UHFFFAOYSA-M gold monochloride Chemical compound [Cl-].[Au+] FDWREHZXQUYJFJ-UHFFFAOYSA-M 0.000 description 1
- 231100000869 headache Toxicity 0.000 description 1
- 208000019622 heart disease Diseases 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 244000144972 livestock Species 0.000 description 1
- 238000001819 mass spectrum Methods 0.000 description 1
- 239000000575 pesticide Substances 0.000 description 1
- 238000004321 preservation Methods 0.000 description 1
- 150000003222 pyridines Chemical class 0.000 description 1
- 238000011897 real-time detection Methods 0.000 description 1
- 239000002689 soil Substances 0.000 description 1
- 230000004083 survival effect Effects 0.000 description 1
- 208000024891 symptom Diseases 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 239000008399 tap water Substances 0.000 description 1
- 235000020679 tap water Nutrition 0.000 description 1
- 230000001988 toxicity Effects 0.000 description 1
- 231100000419 toxicity Toxicity 0.000 description 1
- 229910021642 ultra pure water Inorganic materials 0.000 description 1
- 239000012498 ultrapure water Substances 0.000 description 1
- 235000013311 vegetables Nutrition 0.000 description 1
Classifications
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/75—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated
- G01N21/77—Systems 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
- G01N21/78—Systems 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
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
- G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
- G01N21/33—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using ultraviolet light
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- Physics & Mathematics (AREA)
- Chemical & Material Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Health & Medical Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- Spectroscopy & Molecular Physics (AREA)
- Life Sciences & Earth Sciences (AREA)
- Pathology (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Plasma & Fusion (AREA)
- Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)
- Investigating Or Analysing Materials By The Use Of Chemical Reactions (AREA)
Abstract
The invention discloses a kind of detection methods of pymetrozine in water solution system, based on the gold nanoparticle that pymetrozine can be modified with melamine specific hydrogen bond action occurs for this method, the resonance of gold nanoparticle surface plasma is caused to change, the color and ultravioletvisible absorption intensity, peak value for making solution of gold nanoparticles change, therefore the color change of solution is directly observed by the naked eye, can quickly detect in solution whether contain pymetrozine, have many advantages, such as easy to operate, at low cost, high sensitivity, it is applied widely.The nano material may be implemented to pymetrozine it is real-time, quickly detect.
Description
Technical field
The present invention relates to the detection techniques of pymetrozine, more particularly to a kind of water for quickly, easily identifying complicated component
The detection method of the pymetrozine of low concentration in solution.
Background technique
To reduce, pest and disease damage improves cereal crops, vegetables and fruit Isoquant and quality, chemical insecticide are answered extensively
With.However, remaining insecticide can pollute soil, water environment and food etc., threat is brought to the survival and development of the mankind.
Therefore, the extensive attention that insecticide residues causes people is accurately detected.
Pymetrozine belongs to pyridines or Triazinone insecticide, is completely new non-killing livestock property insecticide, earliest by Switzerland one
Company developed in 1988, which shows excellent control efficiency to the sucking pest of various crop, and right
People, birds and vertebrate toxicity are lower.Nevertheless, Environmental protection mechanism is still classified as pymetrozine potentially
Carcinogen.Excess free enthalpy pymetrozine will lead to the symptoms such as headache, Nausea and vomiting, especially to patients such as hypertension, heart diseases
It endangers bigger.The maximum intake of China's food security standard pymetrozine is 138nM (0.03mg/kg).Therefore, simple and quick inspection
The residual for surveying pymetrozine is extremely important.
At present detection pymetrozine method mainly have high performance liquid chromatography (HPLC, Environmental Pollution and Control, 2008,30,
40-42；Pesticide Science journal, 2011,13,547-550), liquid phase-mass spectrum be used in conjunction method (J.Agric.Food Chem.2008,56,
6851-6856.), gas chromatography (Food Chem.2014,146,448-454), electrochemical process (Anal.Methods,
2015,7,9100-9107), differential pulse polarography (J.Hazard.Mater.2007,141,700-706) etc., though these methods
It is so safe and reliable, but detection process is complicated, and consuming time is long.Up to the present, only two documents, which have been registered, utilizes gold nano
Particle colorimetric detection pymetrozine, but its detection limit for height, sensitive difference, selectively bad (Appl.Mech.Mater.2011,117,
958-961；Micro Nano Lett.2010,5,304-308).Since these detection liquid synthesis processes are complicated, poor repeatability,
The method for quick, the timely on-site test of pymetrozine for realizing aqueous solution is caused to be difficult to realize.
The present invention is directed to the deficiency of above-mentioned detection method, modifies gold nano grain using melamine, is lured based on pymetrozine
Gold nano grain after leading modification is reunited, and color change is caused, to realize the quantitative detection to pymetrozine.Detection of the invention
Method has the characteristics that simple, quick, selectivity is high, sensitivity is good.
Summary of the invention
The problem to be solved in the present invention is for the above technical problems, to invent a kind of quick, accurate and easy inspection
The method for measuring pymetrozine in aqueous solution, this method are applicable not only to the detection of pymetrozine in aqueous solution, and can be used to examine
Pymetrozine in survey fruit juice, green tea solution.
The present invention solves the technical solution that above-mentioned technical problem is taken are as follows: a method of detection pymetrozine, using three
The amine-modified gold nanoparticle of paracyanogen, prepares the gold nanoparticle of functionalization, can be occurred with melamine by pymetrozine specific
Hydrogen bond action so as to cause gold nanoparticle reunion and solution colour is changed, cause gold nanoparticle surface etc.
The peak position and absorption intensity of ion resonance absorption peak change (Fig. 1), realize in aqueous solution pymetrozine it is quick, simple
Just, accurate detection.
A kind of method of quickly detection pymetrozine provided by the invention, includes the following steps:
(1) certain density aqueous solution of chloraurate is added in round-bottomed flask, is heated with stirring to boiling, rapidly joins reduction
After a certain period of time, specific morphology and the gold nanoparticle aqueous solution with a certain size size is made in agent, reaction；
(2) in the case of stirring, it is added dropwise in the gold nanoparticle aqueous solution made from step (1) certain density
Melamine solution, reaction is after a certain period of time up to the functionalization gold nanoparticle aqueous solution of melamine modification；
(3) the functionalization gold nanoparticle aqueous solution conduct for taking melamine made from two parts of isometric steps (2) to modify
Detect liquid；Prepare the aqueous solution solution as a comparison without pymetrozine, by comparative solution and with comparative solution it is isometric to
Detection solution be separately added into two parts described in detection liquid, form the first mixed liquor and the second mixed liquor；
(4) color of the second mixed liquor and the first mixed liquor is compared, color change, then exist in solution to be detected if it exists
Pymetrozine, color change, then be not present pymetrozine if it does not exist in solution to be detected, alternatively, comparison the second mixed liquor and first
The ultravioletvisible absorption intensity of mixed liquor, peak value, if its ultravioletvisible absorption intensity, peak value change, solution to be detected
In there are pymetrozines, if there is no variations, pymetrozine is not present in solution to be detected.
Preferably, if the figure for being able to reflect pymetrozine concentration and solution colour variation relation in solution can be provided
Piece, then the solution colour variation picture and the picture of the standard of the second mixed liquor that can be obtained through the invention compare,
To obtain the concentration of pymetrozine in the second mixed liquor.The picture preparation method of the standard is as follows:
A series of aqueous solution of different pymetrozine concentration is prepared first, in accordance with the preparation method of second mixed liquor, point
The color change of gold nanoparticle caused by the pymetrozine of various concentration Fan Ying not be observed, in this, as colorimetric after a period of time
Standard card.
In above scheme, it is preferable that the concentration of aqueous solution of chloraurate described in step (1) is 1~5mM, and the reaction time is
10~30min.
Preferably, the concentration of melamine solution described in step (2) is 1~5 μM, and the reaction time is 10~30min.
Preferably, the reducing agent is one of sodium borohydride, sodium citrate, potassium citrate or several.
Preferably, the pH range of the functionalization gold nanoparticle aqueous solution of the melamine modification is between 3~6.5.
Preferably, the solution to be detected is that polymer solution in water, lake water solution or foodstuff samples obtain after treatment
Sample solution.
It is further preferred that the sample solution that the foodstuff samples obtain after treatment is green tea or cider (figure
2)。
In conclusion this method is based on reuniting the present invention provides a kind of method for detecting pymetrozine in aqueous solution
Mechanism can form Au-N key using melamine with gold nanoparticle, and pymetrozine can occur specifically with melamine
Hydrogen bond action, so that gold nanoparticle is due to reunion, solution colour changes, and causes gold nanoparticle surface plasma resonance
The peak position and absorption intensity of absorption peak change (Fig. 1), therefore, are directly carried out using naked eyes and UV, visible light spectrophotometric
Determine, can be quickly detected from solution and whether contain pymetrozine, realize in solution pymetrozine it is quick, easy, real-time
Detection.
Preferably, the substance for participating in reaction is that chemistry is pure.
Compared with the prior art, the advantages of the present invention are as follows: the detection method of pymetrozine provided by the invention is easy to operate
Conveniently, it detects quick, low in cost, high sensitivity and can operate on the spot at the scene, the quick inspection suitable for food safety
It surveys, monitors the detection of pymetrozine in domestic water and the various water samples obtained after treatment, be with a wide range of applications.
Detailed description of the invention
Fig. 1 is the uv absorption spectra of functionalization gold nanoparticle aqueous solution of the invention；Wherein (a) is melamine
Gold nanoparticle aqueous solution ultra-violet absorption spectrum after modification；It (b) is the gold nano after the melamine modification containing pymetrozine
Particle aqueous solution ultra-violet absorption spectrum；
Fig. 2 be tap water, lake water, in green tea and cider solution pymetrozine detection picture；Wherein PYM is pymetrozine
Abbreviation.
Specific embodiment
The present invention is further described below by specific embodiment, but does not limit the contents of the present invention.
Embodiment 1
(1) preparation of the gold nanoparticle of the reduction of sodium citrate of melamine modification
(a) preparation of gold nano grain, 10mL 5mM AuCl3·HCl·4H2It is ultrapure that 85mL is added in O under agitation
It in water, is heated to boiling, rapidly joins the sodium citrate solution that 5mL mass fraction is 1%, continue heating stirring to solution colour
It is become colorless by light yellow, after eventually becoming claret, stops heating stirring, standing is cooled to room temperature, is put into 4 DEG C of refrigerator
It saves；
(b) the gold nanoparticle aqueous solution prepared in 20mL step (a) is taken, under agitation, the three of 4 μM are added dropwise dropwise
Paracyanogen amine aqueous solution continues to stir 10min, can obtain the solution of gold nanoparticles of the reduction of sodium citrate of melamine modification, and
As detection solution；
(2) in solution pymetrozine detection
(a) reduction of sodium citrate of two parts of isometric melamine modifications is taken in step (1) detection liquid obtained
Solution of gold nanoparticles；The aqueous solution solution as a comparison without pymetrozine is prepared, by comparative solution and with comparative solution etc.
The solution to be detected of volume is separately added into the solution of gold nanoparticles of the reduction of sodium citrate of two parts of melamines modification
In, form the first mixed liquor and the second mixed liquor；
(b) after reacting 10min, the color of the second mixed liquor and the first mixed liquor is compared, color change, then to be checked if it exists
There are pymetrozines in survey solution, and color change, then be not present pymetrozine if it does not exist in solution to be detected, alternatively, comparison second
Mixed liquor and the ultravioletvisible absorption intensity of the first mixed liquor, peak value, if its ultravioletvisible absorption intensity, peak value change,
Then there are pymetrozines in solution to be detected, if pymetrozine is not present in solution to be detected there is no variation.
Embodiment 2
(1) preparation of the gold nanoparticle of the sodium borohydride reduction of melamine modification
(a) preparation of gold nano grain is added to 4mL 1mM gold chloride in 94mL ultrapure water, is heated to boiling, quickly
The sodium borohydride that 2mL 0.1M is newly configured, which is added, can be made the solution of gold nanoparticles of claret after reacting 20min；
(b) solution of gold nanoparticles prepared in 70mL step (a) is taken, under agitation, 4.0 μ of 20mL is added dropwise dropwise
The melamine solution of M continues to stir 30min, and the gold nanoparticle that can obtain the sodium borohydride reduction of melamine modification is molten
Liquid, and as detection solution；
(2) in solution pymetrozine detection
(a) sodium borohydride reduction of two parts of isometric melamine modifications is taken in step (1) detection liquid obtained
Solution of gold nanoparticles；The aqueous solution solution as a comparison without pymetrozine is prepared, by comparative solution and with comparative solution etc.
The solution to be detected of volume is separately added into the solution of gold nanoparticles of the sodium borohydride reduction of two parts of melamines modification
In, form the first mixed liquor and the second mixed liquor；
(b) after reacting 25min, the color of the second mixed liquor and the first mixed liquor is compared, color change, then to be checked if it exists
There are pymetrozines in survey solution, and color change, then be not present pymetrozine if it does not exist in solution to be detected, alternatively, comparison second
Mixed liquor and the ultravioletvisible absorption intensity of the first mixed liquor, peak value, if its ultravioletvisible absorption intensity, peak value change,
Then there are pymetrozines in aqueous solution to be detected, if pymetrozine is not present in aqueous solution to be detected there is no variation.
Embodiment 3
(1) preparation of the gold nanoparticle of the potassium citrate reduction of melamine modification
(a) preparation of gold nano grain, by 10mL 3mM AuCl3·HCl·4H2It is super that 85mL is added in O under agitation
It in pure water, is heated to boiling, rapidly joins the potassium citrate solution that 5mL mass fraction is 1%, continue heating stirring to solution face
Color is become colorless by light yellow, after eventually becoming claret, stops heating stirring, and standing is cooled to room temperature, and is put into 4 DEG C of refrigerator
Middle preservation；
(b) solution of gold nanoparticles prepared in 70mL step (a) is taken, under agitation, 4.0 μ of 20mL is added dropwise dropwise
The melamine solution of M continues to stir 20min, and the gold nanoparticle that can obtain the potassium citrate reduction of melamine modification is molten
Liquid, and as detection solution；
(2) in solution pymetrozine detection
(a) the potassium citrate reduction of two parts of isometric melamine modifications is taken in step (1) detection liquid obtained
Solution of gold nanoparticles；The aqueous solution solution as a comparison without pymetrozine is prepared, by comparative solution and with comparative solution etc.
The solution to be detected of volume is separately added into the solution of gold nanoparticles of the potassium citrate reduction of two parts of melamines modification
In, form the first mixed liquor and the second mixed liquor；
(b) after reacting 20min, the color of the second mixed liquor and the first mixed liquor is compared, color change, then to be checked if it exists
There are pymetrozines in survey solution, and color change, then be not present pymetrozine if it does not exist in solution to be detected, alternatively, comparison second
Mixed liquor and the ultravioletvisible absorption intensity of the first mixed liquor, peak value, if its ultravioletvisible absorption intensity, peak value change,
Then there are pymetrozines in solution to be detected, if pymetrozine is not present in solution to be detected there is no variation.
Embodiment 4
(1) preparation of the gold nanoparticle for the reduction of sodium citrate that the melamine that pH is 3 is modified
The solution of gold nanoparticles 20mL for the reduction of sodium citrate that melamine is modified in step (1) in Example 1, adds
Entering suitable hydrochloric acid solution to adjust pH is 3, and as detection solution；
(2) in solution pymetrozine detection
The sodium citrate that the melamine that two parts of isometric pH are 3 is modified is measured in step (1) detection liquid obtained
The solution of gold nanoparticles of reduction；Prepare the aqueous solution solution as a comparison without pymetrozine, by comparative solution and with comparison
The isometric aqueous solution to be detected of solution is separately added into the reduction of sodium citrate that the melamine that two parts of pH are 3 is modified
In solution of gold nanoparticles, the first mixed liquor and the second mixed liquor are formed；
After reacting 30min, the color of the second mixed liquor and the first mixed liquor is compared, color change, then to be detected if it exists
There are pymetrozine in aqueous solution, color change, then be not present pymetrozine if it does not exist in aqueous solution to be detected, alternatively, comparison the
Two mixed liquors and the ultravioletvisible absorption intensity of the first mixed liquor, peak value, if its ultravioletvisible absorption intensity, peak value become
Change, then there are pymetrozines in aqueous solution to be detected, if pymetrozine is not present in aqueous solution to be detected there is no variation.
Embodiment 5
(1) preparation of the gold nanoparticle for the reduction of sodium citrate that the melamine that pH is 4 is modified
The solution of gold nanoparticles 20mL for the reduction of sodium citrate that melamine is modified in step (1) in Example 1, adds
Entering suitable hydrochloric acid solution to adjust pH is 4, and as detection solution；
(2) in solution pymetrozine detection
The sodium citrate that the melamine that two parts of isometric pH are 4 is modified is measured in step (1) detection liquid obtained
The solution of gold nanoparticles of reduction；Prepare the aqueous solution solution as a comparison without pymetrozine, by comparative solution and with comparison
The isometric aqueous solution to be detected of solution is separately added into the reduction of sodium citrate that the melamine that two parts of pH are 4 is modified
In solution of gold nanoparticles, the first mixed liquor and the second mixed liquor are formed；
After reacting 15min, the color of the second mixed liquor and the first mixed liquor is compared, color change, then to be detected if it exists
There are pymetrozine in aqueous solution, color change, then be not present pymetrozine if it does not exist in aqueous solution to be detected, alternatively, comparison the
Two mixed liquors and the ultravioletvisible absorption intensity of the first mixed liquor, peak value, if its ultravioletvisible absorption intensity, peak value become
Change, then there are pymetrozines in aqueous solution to be detected, if pymetrozine is not present in aqueous solution to be detected there is no variation.
Embodiment 6
(1) preparation of the gold nanoparticle for the reduction of sodium citrate that the melamine that pH is 5 is modified
The solution of gold nanoparticles 20mL for the reduction of sodium citrate that melamine is modified in step (1) in Example 1, adds
Entering suitable hydrochloric acid solution to adjust pH is 5, and as detection solution；
(2) in solution pymetrozine detection
The sodium citrate that the melamine that two parts of isometric pH are 5 is modified is measured in step (1) detection liquid obtained
The solution of gold nanoparticles of reduction；Prepare the aqueous solution solution as a comparison without pymetrozine, by comparative solution and with comparison
The isometric aqueous solution to be detected of solution is separately added into the reduction of sodium citrate that the melamine that two parts of pH are 5 is modified
In solution of gold nanoparticles, the first mixed liquor and the second mixed liquor are formed；
After reacting 15min, the color of the second mixed liquor and the first mixed liquor is compared, color change, then to be detected if it exists
There are pymetrozine in aqueous solution, color change, then be not present pymetrozine if it does not exist in aqueous solution to be detected, alternatively, comparison the
Two mixed liquors and the ultravioletvisible absorption intensity of the first mixed liquor, peak value, if its ultravioletvisible absorption intensity, peak value become
Change, then there are pymetrozines in aqueous solution to be detected, if pymetrozine is not present in aqueous solution to be detected there is no variation.
Embodiment 7
(1) preparation of the gold nanoparticle for the reduction of sodium citrate that the melamine that pH is 6 is modified
The solution of gold nanoparticles 20mL for the reduction of sodium citrate that melamine is modified in step (1) in Example 1, adds
Entering suitable hydrochloric acid solution to adjust pH is 6, and as detection solution；
(2) in solution pymetrozine detection
The sodium citrate that the melamine that two parts of isometric pH are 6 is modified is measured in step (1) detection liquid obtained
The solution of gold nanoparticles of reduction；Prepare the aqueous solution solution as a comparison without pymetrozine, by comparative solution and with comparison
The isometric aqueous solution to be detected of solution is separately added into the reduction of sodium citrate that the melamine that two parts of pH are 6 is modified
In solution of gold nanoparticles, the first mixed liquor and the second mixed liquor are formed；
After reacting 15min, the color of the second mixed liquor and the first mixed liquor is compared, color change, then to be detected if it exists
There are pymetrozine in aqueous solution, color change, then be not present pymetrozine if it does not exist in aqueous solution to be detected, alternatively, comparison the
Two mixed liquors and the ultravioletvisible absorption intensity of the first mixed liquor, peak value, if its ultravioletvisible absorption intensity, peak value become
Change, then there are pymetrozines in aqueous solution to be detected, if pymetrozine is not present in aqueous solution to be detected there is no variation.
Embodiment 8
(1) preparation of the gold nanoparticle for the reduction of sodium citrate that the melamine that pH is 6.5 is modified
The solution of gold nanoparticles 20mL for the reduction of sodium citrate that melamine is modified in step (1) in Example 1, adds
Entering suitable hydrochloric acid solution to adjust pH is 6.5, and as detection solution；
(2) in solution pymetrozine detection
The citric acid that the melamine that two parts of isometric pH are 6.5 is modified is measured in step (1) detection liquid obtained
The solution of gold nanoparticles of sodium reduction；Prepare the aqueous solution solution as a comparison without pymetrozine, by comparative solution and with it is right
The to be detected aqueous solution more isometric than solution is separately added into the sodium citrate for the melamine modification that two parts of pH are 6.5 also
In former solution of gold nanoparticles, the first mixed liquor and the second mixed liquor are formed；
After reacting 15min, the color of the second mixed liquor and the first mixed liquor is compared, color change, then to be detected if it exists
There are pymetrozine in aqueous solution, color change, then be not present pymetrozine if it does not exist in aqueous solution to be detected, alternatively, comparison the
Two mixed liquors and the ultravioletvisible absorption intensity of the first mixed liquor, peak value, if its ultravioletvisible absorption intensity, peak value become
Change, then there are pymetrozines in aqueous solution to be detected, if pymetrozine is not present in aqueous solution to be detected there is no variation.
Embodiment 9
The detection of pymetrozine in polymer solution in water
The citric acid of two parts of isometric melamine modifications is measured in Example 1 in step (1) detection liquid obtained
The solution of gold nanoparticles of sodium reduction；Prepare the polymer solution in water solution as a comparison without pymetrozine, by comparative solution and
Isometric polymer solution in water to be detected is separately added into the sodium citrate of two parts of melamines modification also with comparative solution
In former solution of gold nanoparticles, the first mixed liquor and the second mixed liquor are formed；
After reacting 25min, the color of the second mixed liquor and the first mixed liquor is compared, color change, then to be detected if it exists
There are pymetrozines in polymer solution in water, and color change, then be not present pymetrozine if it does not exist in polymer solution in water to be detected, or
Person compares the second mixed liquor and the ultravioletvisible absorption intensity of the first mixed liquor, peak value, if its ultravioletvisible absorption intensity, peak
Value changes, then there are pymetrozines in polymer solution in water to be detected, if there is no variation, in polymer solution in water to be detected
There is no pymetrozines.
Embodiment 10
The detection of pymetrozine in lake water
The citric acid of two parts of isometric melamine modifications is measured in Example 1 in step (1) detection liquid obtained
The solution of gold nanoparticles of sodium reduction；Prepare the lake water solution as a comparison without pymetrozine, by comparative solution and with comparison
The isometric lake water to be detected of solution is separately added into Jenner's grain of rice of the reduction of sodium citrate of two parts of melamines modification
In sub- solution, the first mixed liquor and the second mixed liquor are formed；
After reacting 20min, the color of the second mixed liquor and the first mixed liquor is compared, color change, then to be detected if it exists
There are pymetrozines in lake water, and color change, then be not present pymetrozine if it does not exist in lake water to be detected, alternatively, comparison second is mixed
Liquid and the ultravioletvisible absorption intensity of the first mixed liquor, peak value are closed, if its ultravioletvisible absorption intensity, peak value change,
There are pymetrozines in lake water to be detected, if pymetrozine is not present in lake water to be detected there is no variation.
Embodiment 11
(1) preparation of green tea solution
A little green tea is taken, 100 DEG C of water is added, 10min is stood, takes upper layer aqueous solution into a beaker, be cooled to room temperature,
It is filtered using 0.22 μM of filter membrane, it is spare to obtain green tea solution.
(2) in green tea pymetrozine detection
The citric acid of two parts of isometric melamine modifications is measured in Example 1 in step (1) detection liquid obtained
The solution of gold nanoparticles of sodium reduction；Prepare the green tea solution as a comparison without pymetrozine, by comparative solution and with comparison
The isometric green tea solution to be detected of solution is separately added into the Jenner of the reduction of sodium citrate of two parts of melamines modification
In rice corpuscles solution, the first mixed liquor and the second mixed liquor are formed；
After reacting 20min, the color of the second mixed liquor and the first mixed liquor is compared, color change, then to be detected if it exists
There are pymetrozines in green tea, and color change, then be not present pymetrozine if it does not exist in green tea to be detected, alternatively, comparison second is mixed
Liquid and the ultravioletvisible absorption intensity of the first mixed liquor, peak value are closed, if its ultravioletvisible absorption intensity, peak value change,
There are pymetrozines in green tea to be detected, if pymetrozine is not present in green tea to be detected there is no variation.
Embodiment 11
(1) preparation of cider solution
Apple is enucleated, is squeezed the juice with juice extractor, fruit juice is put into centrifugation (8000rpm) 30min in centrifuge tube, is taken
Clear liquid is filtered using 0.22 μM of filter membrane, it is spare to obtain cider.
(2) in cider pymetrozine detection
The sodium citrate of two parts of isometric melamine modifications is taken in Example 1 in step (1) detection liquid obtained
The solution of gold nanoparticles of reduction；Prepare the cider solution as a comparison without pymetrozine, by comparative solution and with comparison
The isometric cider to be detected of solution is separately added into the gold nano of the reduction of sodium citrate of two parts of melamines modification
In particle solution, the first mixed liquor and the second mixed liquor are formed；
After reacting 20min, the color of the second mixed liquor and the first mixed liquor is compared, color change, then to be detected if it exists
There are pymetrozine in cider, color change, then be not present pymetrozine if it does not exist in cider to be detected, alternatively, comparison the
Two mixed liquors and the ultravioletvisible absorption intensity of the first mixed liquor, peak value, if its ultravioletvisible absorption intensity, peak value become
Change, then there are pymetrozines in cider to be detected, if pymetrozine is not present in cider to be detected there is no variation.
Technical solution of the present invention is described in detail in embodiment described above, it should be understood that the above is only
It for specific embodiments of the present invention, is not intended to restrict the invention, all any modifications made in spirit of the invention
With improve etc., should all be included in the protection scope of the present invention.
Claims (7)
1. a kind of method of quickly detection pymetrozine, this method is using gold nanoparticle as main body, on Gold nanoparticle surface
Melamine is modified, the gold nanoparticle of functionalization is prepared, the gold nanoparticle based on functionalization realizes the quick inspection of pymetrozine
It surveys, which is characterized in that specific detecting step is as follows:
(1) certain density aqueous solution of chloraurate is added in round-bottomed flask, is heated with stirring to boiling, rapidly joins reducing agent,
After a certain period of time, gold nanoparticle aqueous solution is made in reaction；
(2) in the case of stirring, certain density trimerization is added dropwise in the gold nanoparticle aqueous solution made from step (1)
The functionalization gold nanoparticle aqueous solution of melamine modification is made in cyanamide solution, reaction after a certain period of time；
(3) the functionalization gold nanoparticle aqueous solution for taking melamine made from two parts of isometric steps (2) to modify is as detection
Liquid；Prepare the aqueous solution solution as a comparison without pymetrozine, by comparative solution and with isometric to be detected of comparative solution
Solution is separately added into two parts of detection liquid, forms the first mixed liquor and the second mixed liquor；
(4) color of the second mixed liquor and the first mixed liquor is compared, if it exists color change, then there are pyrrole aphids in solution to be detected
Ketone, color change, then be not present pymetrozine if it does not exist in solution to be detected, alternatively, the second mixed liquor of comparison is mixed with first
The ultravioletvisible absorption intensity of liquid, peak value are deposited in solution to be detected if its ultravioletvisible absorption intensity, peak value change
In pymetrozine, if pymetrozine is not present in solution to be detected there is no variation.
2. a kind of method of quickly detection pymetrozine as described in claim 1, which is characterized in that the gold of chlorine described in step (1)
The concentration of aqueous acid is 1~5mM, and the reaction time is 10~30min.
3. a kind of method of quickly detection pymetrozine as described in claim 1, which is characterized in that trimerization described in step (2)
The concentration of cyanamide solution is 1~5 μM, and the reaction time is 10~30min.
4. a kind of method of quickly detection pymetrozine as described in claim 1, which is characterized in that the reducing agent is boron hydrogen
Change one of sodium, sodium citrate, potassium citrate or several.
5. a kind of method of quickly detection pymetrozine as described in claim 1, which is characterized in that the melamine modification
The pH range of functionalization gold nanoparticle aqueous solution is between 3~6.5.
6. a kind of method of quickly detection pymetrozine as described in claim 1, which is characterized in that the solution to be detected is certainly
Carry out aqueous solution, the sample solution that lake water solution or foodstuff samples obtain after treatment.
7. a kind of method of quickly detection pymetrozine as claimed in claim 6, which is characterized in that the foodstuff samples are at
The sample solution obtained after reason is green tea solution or cider.
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| CN103645178A (en) * | 2013-09-12 | 2014-03-19 | 华中师范大学 | On-site detection and separation technologies of imidacloprid |
| CN105445259A (en) * | 2015-11-10 | 2016-03-30 | 宁波大学 | Method for quickly detecting clenbuterol based on functionalized gold nanoparticles |
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| CN103645178A (en) * | 2013-09-12 | 2014-03-19 | 华中师范大学 | On-site detection and separation technologies of imidacloprid |
| CN105445259A (en) * | 2015-11-10 | 2016-03-30 | 宁波大学 | Method for quickly detecting clenbuterol based on functionalized gold nanoparticles |
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