CN109682801A - A kind of method and application synthesizing detection melamine based on nanogold - Google Patents
A kind of method and application synthesizing detection melamine based on nanogold Download PDFInfo
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- CN109682801A CN109682801A CN201811609752.2A CN201811609752A CN109682801A CN 109682801 A CN109682801 A CN 109682801A CN 201811609752 A CN201811609752 A CN 201811609752A CN 109682801 A CN109682801 A CN 109682801A
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- G—PHYSICS
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- 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
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- 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
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Abstract
The invention discloses a kind of methods and application that detection melamine is synthesized based on nanogold.Present inventors discovered that melamine molecule can influence the absorbance change that nanogold generates particle, in no melamine, reducing agent restores gold chloride, produces claret nano-Au solution, which has very high absorbance at 520nm；In the presence of melamine, reducing agent restores gold chloride, and the nano-Au solution color of generation is thin out, and solution absorbance value at 520nm reduces.With the increase of content of melamine, solution colour is more shallow, and absorbance value of the solution at 520nm is smaller；Using color variation can qualitative or half-quantitative detection melamine content, can be with the content of quantitative detection melamine using UV-visible spectrometer.In turn, the present invention also provides a kind of colorimetric methods of quickly detection melamine.This method is simple, cheaply, quickly, and high sensitivity, the quick detection suitable for micro melamine.
Description
Technical field
The present invention relates to technical field of food detection, in particular to a kind of side that detection melamine is synthesized based on nanogold
Method and application.
Background technique
On September 13rd, 2008, China national food quality supervision inspection center point out that melamine belongs to industrial chemicals,
It is not allow to be added in food.Melamine (Melamine, chemical formula: C3N3(NH2)3), it is a kind of triazines nitrogen-containing hetero
Ring organic compound, nitrogen quantity can reach 66%.Method, liquid matter method, high-efficient liquid phase color currently, the method for detection melamine is had good manners
The methods of spectrometry, enzyme-linked immunosorbent assay, colloidal gold immunity chromatography.These methods have good sensitivity and specificity,
But expensive instrument, reagent and cumbersome operating procedure are needed, and take time and effort.Therefore, a kind of simple and quick inspection is studied
The method for surveying melamine has great importance.
Summary of the invention
The primary purpose of the present invention is that the shortcomings that overcoming the prior art and deficiency, provide a kind of based on nanogold synthesis inspection
The method for surveying melamine.
Another object of the present invention is to provide the applications of the above-mentioned method that detection melamine is synthesized based on nanogold.
The purpose of the invention is achieved by the following technical solution: a kind of side synthesizing detection melamine based on nanogold
Method includes the following steps:
(1) melamine solution of several various concentrations is mixed with the solution containing gold chloride, adds reducing agent,
Reaction system I is obtained, reacts, obtains the reaction product of known concentration；By the stoste of solution to be measured or dilution and contain chlorine gold
The solution mixing of acid, adds reducing agent, obtains reaction system II, react, obtain solution reaction product to be measured；
(2) color according to the reaction product of known concentration, judges whether contain melamine in solution reaction product to be measured
Amine, judgment criteria are as follows: if the face of the reaction product for the known concentration that the color of solution reaction product to be measured and melamine are 0
Form and aspect at that time, indicate solution to be measured without melamine；If the color of solution reaction product to be measured is known to 0 than melamine
The reaction product of concentration it is of light color when, indicate to contain melamine in solution to be measured；
(3) step (1) is obtained into the reaction product of known concentration and solution reaction product to be measured detects under phase co-wavelength；
The detected value of the reaction product of known concentration is made into standard curve, the detection of establishing criteria curve and solution reaction product to be measured
Value, obtains the concentration of the melamine in solution to be measured.
In step (1):
The concentration of melamine is not less than 0.01 μM in the reaction system I；Preferably 0.05 μM, 0.1 μM, 0.5 μM,
1μM、5μM、10μM。
The concentration of the gold chloride be 0.01mM~10mM, preferably 0.01mM, 0.05mM, 0.1mM, 0.5mM, 1mM,
5mM、10mM。
The reducing agent is preferably sodium citrate, citric acid, sodium borohydride and H2NNH2One of or at least two.
The reductant concentration is 0.01mM~1000mM, preferably 1mM~100mM.
The dosage of the reducing agent preferably presses reducing agent: gold chloride=1~100:1 of molar ratio is calculated.
In step (3):
The time of the reaction is 1min~30min, preferably 5min~15min.
The temperature of the reaction be 30 DEG C~100 DEG C, preferably 30 DEG C, 37 DEG C, 40 DEG C, 50 DEG C, 60 DEG C, 70 DEG C, 80 DEG C,
90℃、100℃。
Described synthesizes application of the method for detection melamine in field of food detection based on nanogold.
The present invention has the following advantages and effects with respect to the prior art:
1. the present invention is based on present inventors discovered that melamine molecule can influence the extinction that nanogold generates particle
Degree variation, in no melamine, reducing agent restores gold chloride, produces claret nano-Au solution, which has at 520nm
Very high absorbance；In the presence of melamine, reducing agent restores gold chloride, and the nano-Au solution color of generation is thin out, and solution exists
Absorbance value reduces at 520nm.With the increase of content of melamine, solution colour is more shallow, absorbance of the solution at 520nm
It is worth smaller；Using color variation can qualitative or half-quantitative detection melamine content, can using UV-visible spectrometer
With the content of quantitative detection melamine.
2. the method for the present invention is simple, cheaply, quickly, and sensitive and specificity is high.
3. present invention could apply to medicine, food quickly examine with the every field such as determination techniques, have widely answer
Use prospect.
Detailed description of the invention
Fig. 1 is the solution thereon figure in the presence of no melamine and 10 μM of melamines.
Fig. 2 is the ultraviolet-visible spectrogram of solution in the presence of no melamine and 10 μM of melamines.
Fig. 3 is detection melamine concentration range of linearity figure.
Fig. 4 is selective experimental solutions figure.
Specific embodiment
Present invention will now be described in further detail with reference to the embodiments and the accompanying drawings, but embodiments of the present invention are unlimited
In this.
Embodiment 1
Accurate draw 0.2mL melamine solution (0.1mM) is added in ready 20mL colorimetric cylinder, then toward colorimetric cylinder
Middle addition 0.3mL chlorauric acid solution (1mM), then plus 0.3mL sodium citrate solution (1mM), add water constant volume to 2mL.Water-bath (100
DEG C) heating 5 minutes, it takes out.
As shown in Figure 1, in the present embodiment in the presence of melamine, solution is in colourless, and when no melamine, solution is in
Claret.Therefore melamine can be detected by color change.
As shown in Fig. 2, solution has very weak absorption value at 520nm in the present embodiment in the presence of melamine, when
When without melamine, solution has very strong absorption value at 520nm.Therefore melamine can be detected by instrument quantitative.
Embodiment 2
Accurate draw 0.2mL melamine solution (0.1mM) is added in ready 20mL colorimetric cylinder, then toward colorimetric cylinder
Middle addition 0.3mL chlorauric acid solution (1mM), then plus 0.3mL sodium citrate solution (10mM), add water constant volume to 2mL.Water-bath (100
DEG C) heating 15 minutes, it takes out.
Solution colour is similar to Fig. 1, and in the present embodiment in the presence of melamine, solution is in colourless, when no melamine,
Solution is in claret.Therefore melamine can be detected by color change.
Solution absorbance is similar to Fig. 2, and in the present embodiment in the presence of melamine, solution has very weak at 520nm
Absorption value, when no melamine, solution has very strong absorption value at 520nm.Therefore it can be detected by instrument quantitative
Melamine.
Embodiment 3
Accurate draw 0.2mL melamine solution (0.1mM) is added in ready 20mL colorimetric cylinder, then toward colorimetric cylinder
Middle addition 0.3mL chlorauric acid solution (1mM), then plus 0.3mL citric acid solution (1mM), add water constant volume to 2mL.Water-bath (70 DEG C)
Heating 5 minutes is taken out.
Solution colour is similar to Fig. 1, and in the present embodiment in the presence of melamine, solution is in colourless, when no melamine,
Solution is in claret.Therefore melamine can be detected by color change.
Solution absorbance is similar to Fig. 2, and in the present embodiment in the presence of melamine, solution has very weak at 520nm
Absorption value, when no melamine, solution has very strong absorption value at 520nm.Therefore it can be detected by instrument quantitative
Melamine.
Embodiment 4
Accurate draw 0.2mL melamine solution (0.1mM) is added in ready 20mL colorimetric cylinder, then toward colorimetric cylinder
Middle addition 0.3mL chlorauric acid solution (1mM), then plus 0.3mL sodium borohydride solution (1mM) plus water constant volume to 2mL.Water-bath (30 DEG C)
It 5 minutes, takes out.
Solution colour is similar to Fig. 1, and in the present embodiment in the presence of melamine, solution is in colourless, when no melamine,
Solution is in claret.Therefore melamine can be detected by color change.
Solution absorbance is similar to Fig. 2, and in the present embodiment in the presence of melamine, solution has very weak at 520nm
Absorption value, when no melamine, solution has very strong absorption value at 520nm.Therefore it can be detected by instrument quantitative
Melamine.
Embodiment 5
Accurate absorption 0.2mL melamine solution (0.5 μM, 1 μM, 5 μM, 10 μM, 50 μM, 100 μM), which is added to, to be ready to
20mL colorimetric cylinder in, then into colorimetric cylinder 0.3mL chlorauric acid solution (1mM) is added, then plus 0.3mL sodium citrate solution
(1mM) adds water constant volume to 2mL, wherein final concentration of 0.05 μM, 0.1 μM, 0.5 μM, 1 μM, 5 μM, 10 μM of melamine.Water
(100 DEG C) of bath are heated 5 minutes, are taken out, are detected at 520nm.
As shown in figure 3, solution absorbance at 520nm is lower and lower with the increase of melamine solution concentration, detection
0.05-10 μM of the range of linearity, linear equation y=0.5672-0.0488x, related coefficient 0.9968, detection is limited to 0.01 μM.With
The technology of other nanogold detection melamine is compared, and the detection limit of this method is lower, an order of magnitude lower than other methods, and
And this method, just with the variation of absorbance at 520nm, data processing is simpler.
Embodiment 6
It is accurate respectively to draw 0.2mL lysine solution (0.1mM), 0.2mL cyanuric acid solution (0.1mM), 0.2mL urea
Solution (0.1mM), 0.2mL solution of spermine (0.1mM), are added separately in ready 20mL colorimetric cylinder, respectively again toward colorimetric
In pipe be added 0.3mL chlorauric acid solution (1mM), then plus 0.3mL sodium citrate solution (100mM), add water constant volume to 2mL.Water-bath
(100 DEG C) 15 minutes take out.
As shown in figure 4, solution is in claret in the present embodiment in the presence of other nitrogen substances.It is examined by instrument quantitative
It is close with solution absorbance in the presence of no melamine to survey solution absorbance at 520nm, therefore may determine that this method has
Selectivity well.
The above embodiment is a preferred embodiment of the present invention, but embodiments of the present invention are not by above-described embodiment
Limitation, other any changes, modifications, substitutions, combinations, simplifications made without departing from the spirit and principles of the present invention,
It should be equivalent substitute mode, be included within the scope of the present invention.
Claims (10)
1. a kind of method for synthesizing detection melamine based on nanogold, it is characterised in that include the following steps:
(1) melamine solution of several various concentrations is mixed with the solution containing gold chloride, adds reducing agent, obtains
Reaction system I, reaction, obtains the reaction product of known concentration；By the stoste of solution to be measured or dilution and contain gold chloride
Solution mixing, adds reducing agent, obtains reaction system II, reacts, obtains solution reaction product to be measured；
(2) color according to the reaction product of known concentration, judges whether contain melamine in solution reaction product to be measured, sentences
Disconnected standard is as follows: if the color phase of the reaction product for the known concentration that the color of solution reaction product to be measured is 0 with melamine
At that time, indicate solution to be measured without melamine；If the known concentration that the color of solution reaction product to be measured is 0 than melamine
Reaction product it is of light color when, indicate to contain melamine in solution to be measured；
(3) step (1) is obtained into the reaction product of known concentration and solution reaction product to be measured detects under phase co-wavelength；It will
Know the reaction product of concentration detected value production standard curve, the detected value of establishing criteria curve and solution reaction product to be measured,
Obtain the concentration of the melamine in solution to be measured.
2. the method for synthesizing detection melamine based on nanogold according to claim 1, it is characterised in that: in step (1)
The reducing agent is sodium citrate, citric acid, sodium borohydride and H2NNH2One of or at least two.
3. the method for synthesizing detection melamine based on nanogold according to claim 1, it is characterised in that:
The concentration of melamine is not less than 0.01 μM in reaction system I described in step (1)；
The concentration of gold chloride described in step (1) is 0.01mM~10mM；
Reductant concentration described in step (1) is 0.01mM~1000mM.
4. according to the method for synthesizing detection melamine based on nanogold in claim 3, it is characterised in that:
The concentration of melamine is 0.05 μM, 0.1 μM, 0.5 μM, 1 μM, 5 μM, 10 μM in the reaction system I；
The concentration of the gold chloride is 0.01mM, 0.05mM, 0.1mM, 0.5mM, 1mM, 5mM, 10mM；
The reductant concentration is 1mM~100mM.
5. the method for synthesizing detection melamine based on nanogold according to claim 1, it is characterised in that:
The dosage of reducing agent described in step (1) presses reducing agent: gold chloride=1~100:1 of molar ratio is calculated.
6. the method for synthesizing detection melamine based on nanogold according to claim 1, it is characterised in that: in step (3)
The time of the reaction is 1min~30min.
7. according to the method for synthesizing detection melamine based on nanogold in claim 6, it is characterised in that: the reaction
Time be 5min~15min.
8. the method for synthesizing detection melamine based on nanogold according to claim 1, it is characterised in that: in step (3)
The temperature of the reaction is 30 DEG C~100 DEG C.
9. according to the method for synthesizing detection melamine based on nanogold in claim 8, it is characterised in that: in step (3)
The temperature of the reaction is 30 DEG C, 37 DEG C, 40 DEG C, 50 DEG C, 60 DEG C, 70 DEG C, 80 DEG C, 90 DEG C, 100 DEG C.
10. the method according to any one of claims 1 to 9 for synthesizing detection melamine based on nanogold is detected in field of food
In application.
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101718708A (en) * | 2009-11-25 | 2010-06-02 | 福州大学 | Method for quickly detecting melamine in milk sample based on nanogold |
| CN102109469A (en) * | 2011-03-15 | 2011-06-29 | 中国人民解放军军事医学科学院卫生学环境医学研究所 | Kit and method for detecting melamine by virtue of fast visual colorimetry |
| CN102706814A (en) * | 2012-05-11 | 2012-10-03 | 福建医科大学 | Rapid melamine determination method using bare gold nanoparticles as developing probe |
| CN105911006A (en) * | 2016-06-06 | 2016-08-31 | 盐城工学院 | Gold-silver composite nanoparticle solution, preparation technology and melamine detection method |
| CN108956593A (en) * | 2018-07-27 | 2018-12-07 | 海南大学 | A method of without aptamer nanogold hydrosol Visual retrieval melamine |
-
2018
- 2018-12-27 CN CN201811609752.2A patent/CN109682801A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101718708A (en) * | 2009-11-25 | 2010-06-02 | 福州大学 | Method for quickly detecting melamine in milk sample based on nanogold |
| CN102109469A (en) * | 2011-03-15 | 2011-06-29 | 中国人民解放军军事医学科学院卫生学环境医学研究所 | Kit and method for detecting melamine by virtue of fast visual colorimetry |
| CN102706814A (en) * | 2012-05-11 | 2012-10-03 | 福建医科大学 | Rapid melamine determination method using bare gold nanoparticles as developing probe |
| CN105911006A (en) * | 2016-06-06 | 2016-08-31 | 盐城工学院 | Gold-silver composite nanoparticle solution, preparation technology and melamine detection method |
| CN108956593A (en) * | 2018-07-27 | 2018-12-07 | 海南大学 | A method of without aptamer nanogold hydrosol Visual retrieval melamine |
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Application publication date: 20190426 |