CN107300551A - A kind of melamine visible detection method based on nano Au particle color change - Google Patents
A kind of melamine visible detection method based on nano Au particle color change Download PDFInfo
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- CN107300551A CN107300551A CN201710443825.4A CN201710443825A CN107300551A CN 107300551 A CN107300551 A CN 107300551A CN 201710443825 A CN201710443825 A CN 201710443825A CN 107300551 A CN107300551 A CN 107300551A
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- 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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Abstract
The present invention relates to a kind of melamine visible detection method based on nano Au particle color change, including：Gold chloride is reduced by trisodium citrate and obtains the nano Au particle aqueous solution that concentration is 2.3nmol/L, particle diameter is 15nm；Oligomerization adenylic acid is dissolved in deionized water and obtains nucleosides aqueous acid, the number of adenine is 10 20；Nucleosides aqueous acid is added in the nano Au particle aqueous solution the final concentration of 100nM until oligomerization adenylic acid, incubation at room temperature obtains the detection solution of claret so that oligomerization adenylic acid chain to be assembled on nano Au particle；Dilution obtains the sample solution that sodium salt concentration is less than 0.1M, to sample solution be filtrated to get the sample clarified solution of water white transparency using degerming filter membrane；Sample clarified solution is mixed with the detection solution of claret, observed by the naked eye.The present invention obtains result by direct visual perception, it is easy to accomplish home diagnostic and Site Detection.
Description
Technical field
The present invention relates to food analysis field, and in particular to a kind of melamine based on nano Au particle color change can
Depending on changing detection method.
Background technology
Melamine, chemical formula is C3N3(NH2)3, also known as extract of protein is a kind of organic compound, is used as chemical industry former
Material, it is harmful, it is not useable for food processing or food addition.But in 2008, China much ate the baby of Sanlu milk powder
Youngster is found to suffer from kidney stone, and the dead case of seriously ill infant occurs.Then, these problem milk powder are found containing melamine
Amine.Investigation display, because protein content required in milk acquisition criteria is determined by nitrogen total content, because
This, illegal retailer improves the nitrogen content in milk by adding nitrogenous melamine in milk, is filled so as to reach with secondary
Good purpose.Specifically " malicious milk powder " crisis generates far-reaching influence so that food-safety problem turns into Jiao that the whole society pays close attention to
Point.Although currently the situation of directly addition melamine is contained in milk product, due to upstreams such as food pollutions
The problem of link it is caused melamine pollution still happen occasionally.Therefore, the melamine in quick detection dairy produce also into
For an active demand involved the interests of the state and the people.
Existing melamine detection method includes efficient liquid phase chromatographic analysis, mass spectral analysis etc., but this kind of method is usual
Large scale equipment is relied on, is unfavorable for quick, Site Detection.
The content of the invention
In order to solve that above-mentioned prior art is present can not rapid field detection melamine the problem of, it is contemplated that carrying
For a kind of melamine visible detection method based on nano Au particle color change.
Melamine visible detection method of the present invention based on nano Au particle color change, including：S1, leads to
Cross trisodium citrate reduction gold chloride and obtain the nano Au particle aqueous solution that concentration is 2.3nmol/L, wherein, nano Au particle
Particle diameter is 15nm；S2, oligomerization adenylic acid is dissolved in deionized water and obtains nucleosides aqueous acid, wherein, oligomerization gland
The number of adenine in purine nucleotides is 10-20；S3, nucleosides aqueous acid is added in the nano Au particle aqueous solution directly
To the final concentration of 100nM of oligomerization adenylic acid, it is incubated at room temperature oligomerization adenylic acid chain being assembled into nanogold
The detection solution of claret is obtained on particle；S4, adds deionized water dilution and obtains sodium salt concentration less than 0.1M in the sample
Sample solution, to sample solution be filtrated to get the sample clarified solution of water white transparency using degerming filter membrane；S5, sample is clarified
Liquid is mixed with the detection solution of claret, and whether the color for observing by the naked eye solution is changed into bluish violet.
In detection solution, particle diameter is homogeneously dispersed in solution for 15nm nano Au particle, distance between nano-particle
Larger, claret is integrally presented in solution.Melamine as a kind of compound containing multiple nitrogen-atoms, in the solution in the presence of
The non-covalent that golden nitrogen key is easily formed between nano Au particle is combined, and triggers the aggregation of nano Au particle so that nanogold
Particle is close to each other to form aggregation, and solution is rendered as bluish violet, so as to be in judgement sample using visual color change
It is no to contain melamine.Moreover, the present invention strengthens nanogold by the way that nucleosides aqueous acid is added in the nano Au particle aqueous solution
Stability of the particle in salt-containing solution, in order to which oligomerization adenylic acid chain is assembled into nano Au particle by being incubated
On.In addition, by Sample Dilution, a large amount of protein in sample can be avoided to produce non-spy with unmodified nano Au particle
Different absorption, so as to disturb the combination of melamine and nano Au particle.In addition, contain 3g albumen in generally per 100mL milk,
200mg sodium salt calcium salts, contain 30 micrograms of protein in 0.1mL samples after 100 times of dilution, salinity is less than 0.3mM.It should be understood that
In some cheese products, salinity is limited within 0.1M sodium salts.Nano Au particle, which meets high concentration salt solutions, to be occurred
Aggregation discoloration, therefore may cause false positive in the higher dairy products of detection salt concentration, and the dilution to sample then can be true
Salinity is reduced to the tolerable scope of nano Au particle by guarantor.
The step S1 includes：S11, chromic acid lotion immersion glassware is stayed overnight, and contains greasy dirt on glassware to remove
Stain；And S12, in glassware, aqueous solution of chloraurate and trisodium citrate aqueous solution back flow reaction obtain nano Au particle
The aqueous solution.
Chromic acid lotion in the step S11 in the 100mL concentrated sulfuric acids by being slowly added into 5g potassium bichromates powder and stirring
Dissolving is mixed to prepare.
The step S12 is specially：0.01g gold chlorides are dissolved in 100mL deionized waters, are placed in magnetic agitation
In the flask of son and condensation reflux unit, stir and oil bath heating is to seething with excitement, the concentration for adding Fresh is 10mg/mL lemon
Lemon three sodium water solution 3.5mL of acid, continue to be kept stirring for ebuillition of heated 20 minutes.
By above-mentioned steps S11 and S12, concentration is directly obtained for 2.3nmol/L, and particle diameter is 15nm nano Au particle water
Solution, without diluting or concentrating.
The sequence of oligomerization adenylic acid in the step S2 is 5 '-AAAAAAAAAA-3 '.
The aperture of degerming filter membrane in the step S4 is 0.22 micron.
Sample in the step S4 is commercially available milk.
The step S4 is specially：Dilute commercially available milk 100 and obtain sample solution again, utilize degerming filter membrane and syringe pair
Sample solution be filtrated to get the sample clarified solution of water white transparency.
It should be understood that if extension rate is too small, milky is presented in sample solution, influences follow-up color observation；If
Extension rate is excessive, can substantially reduce melamine concentration, so as to reduce detection sensitivity.Wherein, the dilution operation can be removed
The albumen aggregation of the sample of great quantities of spare in itself is gone, in order to follow-up detection.
The step S5 is specially：0.1 milliliter of sample clarified solution is mixed with 1 milliliter of detection solution, placed about 2 minutes,
Whether the color for observing by the naked eye solution judges whether to contain melamine in commercially available milk by claret is changed into bluish violet.
The detectable limit of the melamine of sample in the step S4 is 0.1mg/L.
Experiment shows：In the reference examples containing concentration for 1mg/L melamine, the color for visually observing solution is changed into
Bluish violet, and in the sample of the melamine containing concentration less than 0.1mg/L, solution remains original claret.
The present invention using nano Au particle it is unique optical property --- the nano Au particle of different aggregation extents is due to table
Face plasma resonance bulk effect and different colors are presented, realize the quick detection based on color change.Obviously, it is this to pass through
Direct visual perception obtains the mode of result, independent of large scale equipment, it is easy to accomplish home diagnostic and Site Detection.In addition, this
Antibody or other biological macromolecular ligand of the detection method of invention independent of specific recognition melamine, due to preparing,
Transport and storage antibody etc. are often more difficult, and therefore, detection method of the invention significantly reduces testing cost.Moreover,
The sensitivity of the method for the present invention has reached the melamine that milk power for infant and young children is limited in the national standard promulgated for 2008
Amine concentrations (1mg/L), and inexpensively, it is quick, convenient, it is not necessary to professional equipment and professional technique, also without poisonous and harmful examination
Agent, therefore be easy to standardize, be commercialized, and promoted the use of in home environment or daily sampling observation.
Embodiment
Presently preferred embodiments of the present invention is given below, and is described in detail.
Embodiment 1
5g potassium bichromates powder is slowly added into the 100mL concentrated sulfuric acids and stirring and dissolving prepares chromic acid lotion, glass is soaked
Vessel are stayed overnight, to remove the oil-containing spot on glassware；
0.01g gold chlorides (traditional Chinese medicines) are dissolved in 100mL deionized waters, are placed in magnetic stir bar and condensing reflux
In the flask of device, stir and oil bath heating is to seething with excitement, the concentration for adding Fresh is 10mg/mL trisodium citrate (state
Medicine) aqueous solution 3.5mL, continues to be kept stirring for ebuillition of heated 20 minutes, obtains the nano Au particle that concentration is 2.3nmol/L water-soluble
Liquid, wherein, the particle diameter of nano Au particle is 15nm；
Sequence is dissolved in deionized water for 5 '-AAAAAAAAAA-3 ' oligomerization adenylic acid and obtains nucleotides
The aqueous solution；
Nucleosides aqueous acid is added in the nano Au particle aqueous solution until oligomerization adenylic acid it is final concentration of
100nM, incubation at room temperature obtains the detection solution of claret so that oligomerization adenylic acid chain to be assembled on nano Au particle；
The commercially available milk of several brands is taken, is divided in pipettor in 2 milliliters of centrifuge tubes, is added in a wherein pipe sample
1mg/L melamines are used as positive control.Then, each sample is diluted 100 times, respectively takes 1 milliliter to be sub-packed in centrifuge tube.Connect down
Come, with the aseptic filtration film with 0.22 micron pore size will dilute after sample filtering once, to remove albumen unnecessary in sample
Matter, obtains the sample clarified solution of water white transparency；
0.1 milliliter of sample clarified solution is taken, is well mixed, after placing two minutes, passes through with 1 milliliter of detection solution in centrifuge tube
Whether the color for visually observing solution judges whether to contain melamine in commercially available milk by claret is changed into bluish violet.
As a result：Claret is still presented in the milk sample for not adding melamine, and with the addition of the sample of melamine
Color is changed into bluish violet.By the test to commercially available six kinds of brand milk samples, as a result show that these samples will not make nanometer
Gold particle solution changes color, illustrates that these milk do not contain this method and can detect the melamine of dosage.
Above-described, only presently preferred embodiments of the present invention is not limited to the scope of the present invention, of the invention is upper
Stating embodiment can also make a variety of changes.What i.e. every claims and description according to the present patent application were made
Simply, equivalent changes and modifications, falls within the claims of patent of the present invention.The present invention not detailed description is
Routine techniques content.
Claims (10)
1. a kind of melamine visible detection method based on nano Au particle color change, it is characterised in that including：
S1, reduces gold chloride by trisodium citrate and obtains the nano Au particle aqueous solution that concentration is 2.3nmol/L, wherein, receive
The particle diameter of rice gold particle is 15nm；
S2, oligomerization adenylic acid is dissolved in deionized water and obtains nucleosides aqueous acid, wherein, oligomerization adenosine
The number of adenine in acid is 10-20；
S3, nucleosides aqueous acid is added in the nano Au particle aqueous solution until oligomerization adenylic acid it is final concentration of
100nM, incubation at room temperature obtains the detection solution of claret so that oligomerization adenylic acid chain to be assembled on nano Au particle；
S4, adds deionized water dilution and obtains the sample solution that sodium salt concentration is less than 0.1M, utilize degerming filter membrane pair in the sample
Sample solution be filtrated to get the sample clarified solution of water white transparency；
S5, sample clarified solution is mixed with the detection solution of claret, and whether the color for observing by the naked eye solution is changed into royal purple
Color.
2. melamine visible detection method according to claim 1, it is characterised in that the step S1 includes：
S11, chromic acid lotion immersion glassware is stayed overnight, to remove the oil-containing spot on glassware；And
S12, in glassware, aqueous solution of chloraurate and trisodium citrate aqueous solution back flow reaction obtain nano Au particle water
Solution.
3. melamine visible detection method according to claim 2, it is characterised in that the chromium in the step S11
Pickle in the 100mL concentrated sulfuric acids by being slowly added into 5g potassium bichromates powder and stirring and dissolving preparation.
4. melamine visible detection method according to claim 2, it is characterised in that the step S12 is specially：
0.01g gold chlorides are dissolved in 100mL deionized waters, are placed in the flask with magnetic stir bar and condensation reflux unit,
Stir and oil bath heating is to seething with excitement, the concentration for adding Fresh is 10mg/mL trisodium citrate aqueous solution 3.5mL, is continued
It is kept stirring for ebuillition of heated 20 minutes.
5. melamine visible detection method according to claim 1, it is characterised in that the oligomerization in the step S2
The sequence of adenylic acid is 5 '-AAAAAAAAAA-3 '.
6. melamine visible detection method according to claim 1, it is characterised in that degerming in the step S4
The aperture of filter membrane is 0.22 micron.
7. melamine visible detection method according to claim 1, it is characterised in that the sample in the step S4
For commercially available milk.
8. melamine visible detection method according to claim 7, it is characterised in that the step S4 is specially：
Dilute commercially available milk 100 and obtain sample solution again, sample solution progress is filtrated to get using degerming filter membrane and syringe colourless
Transparent sample clarified solution.
9. melamine visible detection method according to claim 8, it is characterised in that the step S5 is specially：
By 0.1 milliliter of sample clarified solution with 1 milliliter detection solution mix, placement about 2 minutes, observe by the naked eye solution color whether
Judge whether to contain melamine in commercially available milk by claret is changed into bluish violet.
10. melamine visible detection method according to claim 1, it is characterised in that the sample in the step S4
The detectable limit of this melamine is 0.1mg/L.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201710443825.4A CN107300551A (en) | 2017-06-13 | 2017-06-13 | A kind of melamine visible detection method based on nano Au particle color change |
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| CN201710443825.4A CN107300551A (en) | 2017-06-13 | 2017-06-13 | A kind of melamine visible detection method based on nano Au particle color change |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108872112A (en) * | 2018-07-07 | 2018-11-23 | 北京建筑大学 | The detection method of lead ion |
| CN111537461A (en) * | 2020-05-28 | 2020-08-14 | 武汉科技大学 | Method for detecting adenine and guanine in solution by using boron cluster nanogold |
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|---|---|---|---|---|
| CN101403691A (en) * | 2008-11-14 | 2009-04-08 | 苏州艾杰生物科技有限公司 | Melamine or tricyanic acid measuring method and its reagent kit or test paper strip |
| CN101701259A (en) * | 2009-10-20 | 2010-05-05 | 武汉大学 | Method for detecting melamine based on oligonucleotides-modified nano-gold |
| CN102608073A (en) * | 2012-03-09 | 2012-07-25 | 西南大学 | Quick detection method for melamine in dairy products |
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2017
- 2017-06-13 CN CN201710443825.4A patent/CN107300551A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101403691A (en) * | 2008-11-14 | 2009-04-08 | 苏州艾杰生物科技有限公司 | Melamine or tricyanic acid measuring method and its reagent kit or test paper strip |
| CN101701259A (en) * | 2009-10-20 | 2010-05-05 | 武汉大学 | Method for detecting melamine based on oligonucleotides-modified nano-gold |
| CN102608073A (en) * | 2012-03-09 | 2012-07-25 | 西南大学 | Quick detection method for melamine in dairy products |
Non-Patent Citations (2)
| Title |
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| HUI HUANG等: "Visual detection of melamine in milk samples based on label-free and labeled Gold nanoparticles", 《TALANTA》 * |
| 曹倩等: "寡聚核苷酸标记纳米金可视化检测三聚氰胺", 《分析实验室》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108872112A (en) * | 2018-07-07 | 2018-11-23 | 北京建筑大学 | The detection method of lead ion |
| CN111537461A (en) * | 2020-05-28 | 2020-08-14 | 武汉科技大学 | Method for detecting adenine and guanine in solution by using boron cluster nanogold |
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Application publication date: 20171027 |