CN103323417A - Method for rapidly detecting dicyandiamide in milk based on nanogold visualization - Google Patents
Method for rapidly detecting dicyandiamide in milk based on nanogold visualization Download PDFInfo
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- CN103323417A CN103323417A CN2013102918738A CN201310291873A CN103323417A CN 103323417 A CN103323417 A CN 103323417A CN 2013102918738 A CN2013102918738 A CN 2013102918738A CN 201310291873 A CN201310291873 A CN 201310291873A CN 103323417 A CN103323417 A CN 103323417A
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Abstract
The invention provides a method for rapidly detecting dicyandiamide in milk based on nanogold visualization, and belongs to the food analysis field. The method is characterized in that nanogold is prepared through a process for utilizing gallic acid to reduce chloroauric acid at room temperature. The addition of dicyandiamide in the nano-gold synthesis process causes the aggregation of nano-gold, so the color and the ultraviolet-visible absorption peaks of nano-gold change, and the dicyandiamide can be quantitatively detected through visual observation and an ultraviolet-visible absorption spectrometer. The method has the advantages of simple operation, rapidness, high sensitivity and good selectivity, and can be used in the detection of dicyandiamide in milk.
Description
Technical field
The present invention relates to a kind of Food Safety Analysis method, specifically refer to the mensuration by visual inspection and ultraviolet-visible spectrometer, the content of dicyandiamide in the milk is quantitatively detected.This method belongs to the food analysis field.
Background technology
At the beginning of 2013, New Zealand primary industry section announces, finds in this state's milk and the milk powder to exist the chemical substance dicyandiamide of low toxicity residual.The large bag milk of the New Zealand of Chinese market upper inlet (comprising skimmed milk power, whole milk powder) has accounted for 80% of Chinese general import amount, and New Zealand's dairy products have accounted for about 40% of Chinese import infant food.Yet, for the limiting the quantity of all without standard of dicyandiamide in the food, cause world consumption person's extensive concern and worry in the world.
Dicyandiamide is the dimer of cyanamide, also is the cyano derivative of guanidine.Dicyandiamide is commonly used for raw materials for production and medicine and the dyestuff intermediate of melamine.The New Zealand peasant generally can use dicyandiamide in the pasture, and purpose is to prevent that the harmful fertilizer secondary product such as nitrate from flowing into river or lake, and this has just caused residual medicine to flow in the Contents in Cows, causes the pollution of milk products.
Just because of the blank of dicyandiamide relevant criterion and toxicity Journal of Sex Research, consumer and international market are residual all beyond affordability for detecting dicyandiamide in the milk powder.Therefore, the study on determination method of dicyandiamide content has important theory value and practical significance in the food.
The detection method of dicyandiamide comprises Hydrolyze method, spectrophotometric method, Raman spectrum analysis method, Liquid Chromatography-Mass Spectrometry, high performance liquid chromatography etc. at present.Wherein, high performance liquid chromatography is to detect the common method of dicyandiamide in the food.The method need to be passed through sample extraction, crosses the post purifying, just can analyze after concentrating, and process is loaded down with trivial details and cost is higher, and sample loss is also larger, especially is not suitable for fast-field evaluation and universal.Therefore, in the urgent need to new method quick, easy, accurate, sensitive and that can be used for the Site Detection dicyandiamide.
Summary of the invention
The technical problem to be solved in the present invention is nanometer technology is introduced in the detection application of dicyandiamide, a kind of method based on dicyandiamide in the visual fast detecting milk of nm of gold is provided, and the method has simply, fast, sensitive advantage can be used for on-the-spot food inspection.
For achieving the above object, dicyandiamide method for quick proposed by the invention adopts naked eyes and UV, visible light-spectral analysis to combine, thereby realizes the field quick detection of dicyandiamide.It is characterized in that:
1. at room temperature, prepare nm of gold take gallic acid as reductive agent, adding because of dicyandiamide in the preparation process of nm of gold affects the nanometer state of gold, thereby causes that the color of nm of gold and uv-visible absorption spectra change, and then realizes the visual detection to dicyandiamide.
2. when the preparation nm of gold, the solvent that adopts is 0.01M, the phosphate buffer solution of pH=6.0.Add successively chlorauric acid solution in phosphate buffer, gallic acid solution leaves standstill 5min after shaking up, and observes the variation of solution colour, and measures its ultraviolet-visible light spectrogram.
3. the concentration of gold chloride and gallic acid is respectively 2.0 * 10
-4M and 1.0 * 10
-4M.
4. when not adding dicyandiamide, synthetic nm of gold is in disperse state, and solution presents redness, but after introducing dicyandiamide in the system, the synthetic of nm of gold is affected, and causes nanometer state of gold and color to change.
5. the method relates to the red shift of ultraviolet-visible spectrum maximum absorption band, and the nm of gold that namely is in disperse state has absorption maximum at the 530nm place, and the maximum absorption band of the nm of gold of gathering with the increase of aggregation extent red shift occurs gradually.
6. when processing the ultraviolet-visible spectrum data, the red shift amount of nm of gold maximum absorption band and the content of dicyandiamide are set up quantitative relationship.
The invention has the beneficial effects as follows:
1) one-step synthesis nm of gold at room temperature, and in the building-up process of nm of gold, realize visual detection to dicyandiamide.
2) simple to operate, have preferably selectivity and higher sensitivity.
3) can be applied to the detection of dicyandiamide in the milk.
Description of drawings
Fig. 1 is the effect schematic diagram of dicyandiamide and gallic acid.
Fig. 2 is dicyandiamide content and nm of gold color and ultraviolet-visible spectrum variation diagram.
Fig. 3 is the quantitative detection of dicyandiamide.
Embodiment
1. utilize sodium hydrogen phosphate and sodium dihydrogen phosphate preparation phosphate buffer solution, and configure gold chloride, gallic acid, dicyandiamide solution with intermediate water; Add successively chlorauric acid solution in buffer solution, gallic acid solution leaves standstill 5min after shaking up, and observes the variation of solution colour, and measures its ultraviolet-visible light spectrogram.
2. in buffer solution, add successively chlorauric acid solution, the dicyandiamide solution of variable concentrations, or be added with the milk sample solution of concentration known dicyandiamide, gallic acid solution, leave standstill 5min after shaking up, observe the variation of solution colour, and measure its ultraviolet-visible light spectrogram.
3. the solvent that adopts is 0.01M, the phosphate buffer of pH=6.0, and the concentration of gold chloride and gallic acid is respectively 2.0 * 10
-4M and 1.0 * 10
-4M.
4. when not adding dicyandiamide, synthetic nm of gold is in disperse state, solution presents redness, there is maximum absorption band at the 530nm place on uv-visible absorption spectra, after introducing dicyandiamide in the system, because the interaction (Fig. 1) of dicyandiamide and gallic acid, cause nm of gold to become state of aggregation from disperse state gradually, and along with the aggregation extent of the increase nm of gold of dicyandiamide concentration also increases gradually, the color of the solution becomes purple by redness simultaneously, arrive again blue (Fig. 2), corresponding uv-visible absorption spectra also change (Fig. 2), by measuring the situation of change of nm of gold uv-visible absorption spectra maximum absorption band corresponding wavelength, just can carry out quantitative test (Fig. 3) to dicyandiamide.
The above is described in detail the preferred embodiments of the disclosure and embodiment by reference to the accompanying drawings, but the present invention is not limited to the above-described embodiment and examples, in the ken that those skilled in the art possess, can also make without departing from the inventive concept of the premise various variations.
Claims (7)
1. method based on dicyandiamide in the visual fast detecting milk of nm of gold, it is characterized in that: at room temperature, prepare nm of gold take gallic acid as reductive agent, adding because of dicyandiamide in the preparation process of nm of gold affects the nanometer state of gold, thereby cause that the color of nm of gold and uv-visible absorption spectra change, and then realize the visual detection to dicyandiamide.
2. a kind of method based on dicyandiamide in the visual fast detecting milk of nm of gold as claimed in claim 1 is characterized in that: when the preparation nm of gold, the solvent that adopts is 0.01M, the phosphate buffer solution of pH=6.0.
3. a kind of method based on dicyandiamide in the visual fast detecting milk of nm of gold as claimed in claim 1, it is characterized in that: in phosphate buffer, add successively chlorauric acid solution, gallic acid solution, leave standstill 5min after shaking up, observe the variation of solution colour, and measure its ultraviolet-visible light spectrogram.
4. a kind of method based on dicyandiamide in the visual fast detecting milk of nm of gold as claimed in claim 1, it is characterized in that: the concentration of gold chloride and gallic acid is respectively 2.0 * 10
-4M and 1.0 * 10
-4M.
5. a kind of method based on dicyandiamide in the visual fast detecting milk of nm of gold as claimed in claim 1, it is characterized in that: when not adding dicyandiamide, synthetic nm of gold is in disperse state, solution presents redness, but after introducing dicyandiamide in the system, the synthetic of nm of gold is affected, and causes nanometer state of gold and color to change.
6. a kind of method based on dicyandiamide in the visual fast detecting milk of nm of gold as claimed in claim 1, it is characterized in that: the method relates to the red shift of ultraviolet-visible spectrum maximum absorption band, the nm of gold of namely disperseing has absorption maximum at the 530nm place, and the maximum absorption band of the nm of gold of gathering with the increase of aggregation extent red shift occurs gradually.
7. a kind of method based on dicyandiamide in the visual fast detecting milk of nm of gold as claimed in claim 1, it is characterized in that: when processing the ultraviolet-visible spectrum data, the red shift amount of nm of gold maximum absorption band and the content of dicyandiamide are set up quantitative relationship.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103983594A (en) * | 2014-05-04 | 2014-08-13 | 四川大学 | Method for measuring content of melamine and/or dicyandiamide in dairy products |
| CN104568909A (en) * | 2015-02-10 | 2015-04-29 | 吕志伟 | Method for detecting content of dicyandiamide in milk based on surface enhanced Raman scattering technology |
| CN113552117A (en) * | 2021-06-30 | 2021-10-26 | 中南民族大学 | Atractylodes macrocephala origin tracing method based on nanometer effect visual sensor |
-
2013
- 2013-07-12 CN CN2013102918738A patent/CN103323417A/en active Pending
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103983594A (en) * | 2014-05-04 | 2014-08-13 | 四川大学 | Method for measuring content of melamine and/or dicyandiamide in dairy products |
| CN104568909A (en) * | 2015-02-10 | 2015-04-29 | 吕志伟 | Method for detecting content of dicyandiamide in milk based on surface enhanced Raman scattering technology |
| CN113552117A (en) * | 2021-06-30 | 2021-10-26 | 中南民族大学 | Atractylodes macrocephala origin tracing method based on nanometer effect visual sensor |
| CN113552117B (en) * | 2021-06-30 | 2022-06-17 | 中南民族大学 | Atractylodes macrocephala origin tracing method based on nanometer effect visual sensor |
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Application publication date: 20130925 |