CN101718708A - Method for quickly detecting melamine in milk sample based on nanogold - Google Patents
Method for quickly detecting melamine in milk sample based on nanogold Download PDFInfo
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Abstract
The invention provides a method for quickly detecting melamine in a milk sample based on nanogold, which aims to solve the problems of the high operation requirement, complex detection process, high cost, long time, incapacity of meeting a lot of food test requirements and the like on the detection of the melamine. The method comprises the following steps: performing pretreatment on the milk sample and adding the pretreated milk sample into a nanogold solution; and adopting visual colorimetry to compare the color of the nanogold added with the sample solution with the color in a color standard series and then qualitatively judging whether the milk contains the melamine or not. The color standard series is prepared through the following steps: adding the pretreated milk samples in an identical volume and containing the melamine of different concentrations into the nanogold solution, wherein the content of the nanogold in each sample is consistent; and after color development reaction, obtaining the color standard series. The method has the advantages of low cost, simple and convenient operation and capacity of visually and quickly detecting the melamine in the milk.
Description
Technical field
The invention belongs to melamine detection technique field, more specifically relate to a kind of method based on melamine in the nm of gold fast detecting milk sample.
Background technology
Melamine (melamine) is a kind of triazines nitrogen heterocyclic ring organic compound, is called for short triamine, is commonly called as melamine, extract of protein.As a kind of broad-spectrum Organic Chemicals, the topmost purposes of melamine is that in addition, melamine also is used as fire retardant, water reducer, formaldehyde detersive etc. as the starting material of producing melamine formaldehyde resin (MF).Owing to mainly calculate Protein content in the food indirectly in the food industry by the content of Kjeldahl mensuration nitrogen-atoms, in recent years, melamine is added to the apparent protein content that is used to improve product in food and the feed because of its high nitrogen-containing (66%) by the lawless person.Studies show that melamine has slight toxicity, but long-term take in the calculus that melamine can cause the infringement of reproduction, urinary system and bladder, kidney, and can further bring out carcinoma of urinary bladder.The artificial excessive melamine that mixes caused a lot of pets incident of being poisoned to death, and also therefore broken out the infant and caused the malignant event of kidney stone even death because of having eaten the milk powder that contains melamine.Therefore set up that detection method is very important with the safety of guaranteeing food fast.
Be used for the national standard (standard No.: GB/T 22388-2008) adopt high performance liquid chromatography (HPLC), liquid chromatography-mass spectrography/mass spectroscopy (LC-MS/MS), GC-MS(gas chromatography-mass spectrography) GC-MS) that melamine detects at present, though these methods have higher sensitivity and lower detectability, but need carry out the complicated sample pre-treatment, detection time is longer, instrument costs an arm and a leg, detection cost height is not suitable for the on-site quick screening of melamine in the milk.In the relevant patent of the melamine fast detecting of having announced at present, 200910078299.1 and 200910078300.0), the electrochemical method (patent No.: 200810234859.3 and 200910029572.1) all need rely on the instrument of specialty under professional and technical personnel's operation, just can finish the method for the Raman spectrum (patent No.: to melamine detection.200810202732.3), the test paper (patent No.: 200810197094.0) etc. and be used for pertinent instruments (ZL 200820213241.4), the kit (patent No.: of melamine fast measuring because of its complex structure, manufacturing process is loaded down with trivial details, also is very restricted in actual applications.In addition, be subjected to the influence of biomolecule stability, technician's operation is required than higher based on the immunoreactive immunology detection technology of antigen-antibody.Therefore conventional detection can't satisfy melamine residual detection needs in the food fully.
Summary of the invention
The object of the present invention is to provide a kind of method based on melamine in the nm of gold fast detecting milk sample.Solve in the prior art high to melamine detection operation requirement, the testing process complexity detects the cost height, and detection time is long, can not satisfy the problems such as requirement of a large amount of Food Inspection, method cost of the present invention is low, easy and simple to handle, can visual fast detecting milk in melamine.
Technical scheme of the present invention is mainly two kinds based on the method for melamine in the nm of gold fast detecting milk sample:
One: visual colorimetry
After milk sample carried out pre-treatment, be added to nm of gold, adopt visual colorimetry, solution colour and the color standards series that adds after the nm of gold is compared, whether contain melamine in the qualitative judgement milk; Being prepared as of described color standards series: the milk standard specimen that contains the variable concentrations melamine that adopts equal volume through pre-treatment, it is added in the nano-Au solution, contained nm of gold amount unanimity in each sample after the chromogenic reaction, obtains color standards series.
Two: uv-visible absorption spectra
After milk sample carried out pre-treatment, add nm of gold after solution adopt ultraviolet-visible spectrophotometer to measure absorbance, the absorbance of measuring is introduced the content that the typical curve Equation for Calculating obtains melamine in the milk; Described typical curve equation: the milk standard specimen that contains the variable concentrations melamine that adopts equal volume through pre-treatment, it is added in the nano-Au solution, contained nm of gold amount unanimity in each sample, after the chromogenic reaction, adopt ultraviolet-visible spectrophotometer to be determined at 650nm wavelength and 520nm wavelength place absorbance, will be at the ratio A of 650nm and 520nm place absorbance
650/ A
520As horizontal ordinate, the concentration of melamine is as ordinate, and the drawing standard curve also draws the typical curve equation, and the concentration content range of the melamine that can measure is 0～15.2ppm for liquid milk, is 0～79.8ppm for milk powder; The making scope of typical curve is 0～15.2ppm according to liquid milk, and milk powder is 0～79.8ppm, gets the point of some variable concentrations, measures absorbance at 650nm wavelength and 520nm wavelength place, will be at the ratio A of 650nm and 520nm place absorbance
650/ A
520As horizontal ordinate, the concentration of melamine is as ordinate, and the drawing standard curve also draws the typical curve equation.
Remarkable advantage of the present invention is:
The present invention is based on repulsive force between the citrate negative ion on nm of gold surface make nm of gold can stable existence in aqueous solution, but melamine molecule can reduce the negative charge density on nm of gold surface effectively, repulsive force between the particle reduces, finally cause the gathering of nm of gold, thereby show the principle of the variation of solution colour and ultra-violet absorption spectrum, by milk sample is carried out simple pre-treatment, can be directly used in melamine detection.Influence at interfering material in the actual sample, the present invention removes protein and fat in the actual sample respectively with trichloroacetic acid and chloroform, after centrifugal, add certain amount of alkaline solution and regulate pH to neutral in supernatant, the clarified supernatant that obtains can satisfy the detection requirement.
A kind of method of the present invention based on melamine in the nm of gold fast detecting milk sample; the used nm of gold of this method with the citrate negative ion as protective agent; about 10～the 50nm of nanogold particle diameter; the aqueous solution resonance absorbing peak is about 518nm～540nm, and this nm of gold can be directly as the sensor that detects melamine in the milk sample.
Simple and feasible, the technology maturation of the preparation method of nm of gold of the present invention, and good stability need not nm of gold further modified and promptly can be used for melamine detection;
The present invention requires low to sample pre-treatments, only need simple sample pre-treatments;
Detection speed of the present invention is fast, can finish the pre-treatment and the detection of actual sample about 25 minutes;
The present invention assembles the difference of situation by nm of gold, can change the melamine of indicating variable concentrations by obvious color, can judge by visual inspection whether melamine exceeds standard, can rely on any instrument, therefore it is low, easy and simple to handle to detect cost.
In a word, provided by the invention method is simple, workable, can satisfy requirement of experiment in general laboratory.Method by the nm of gold colorimetric has realized visual melamine quick identification and detection.
Description of drawings
Fig. 1 is that the ultraviolet-visible that the supernatant after the liquid milk of the melamine of the embodiment of the invention 1 adding different quality ratio is handled is assembled nm of gold absorbs spectrogram.
Fig. 2 is that supernatant after the liquid milk of the embodiment of the invention 1 melamine that adds the different quality ratio is handled is to the ratio (A of nm of gold in 650nm and 520nm absorbance
650/ A
520) influence.
Fig. 3 is that supernatant after the liquid milk of the embodiment of the invention 1 melamine that adds the different quality ratio is handled is to the influence of nm of gold change color.
Fig. 4 is that the ultraviolet-visible that the supernatant after the milk powder of the melamine of the embodiment of the invention 2 adding different quality ratios is handled is assembled nm of gold absorbs spectrogram.
Fig. 5 is that supernatant after the milk powder of the embodiment of the invention 2 melamine that adds the different quality ratios is handled is to the ratio (A of nm of gold in 650nm and 520nm absorbance
650/ A
520) influence.
Fig. 6 is that supernatant after the milk powder of the embodiment of the invention 2 melamine that adds the different quality ratios is handled is to the influence of nm of gold change color.
Embodiment
Milk sample carries out pre-treatment: add trichloroacetic acid and chloroform in milk.Liquid milk: add 0.45mL trichloroacetic acid (10%) and 0.625mL chloroform in every gram liquid milk; Milk powder: add 3.33mL trichloroacetic acid (10%) and 2mL chloroform in every gram milk powder respectively; Centrifuging after the sonicated (200W sonicated 15 minutes after 13000rpm centrifugal 6 minutes) removes deproteinize and fat, the supernatant of gained transfers to pH 7.0-8.0 with the 1M sodium carbonate liquor with its pH, further remove sediment by the method for centrifuging (the centrifugal 1min of 3000rpm) again, get the milk sample after supernatant is pre-treatment; The pre-treatment of described milk standard specimen is identical with the milk sample pre-treatment.
When the detection thing is milk powder, milk powder is dissolved in the water, handle according to the step of described milk sample pre-treatment again.
Nano-Au solution with milk sample after the 0.2mL pre-treatment or standard specimen adding 0.1mL; Being prepared as of described nano-Au solution: the method that adopts sodium citrate reduction gold chloride, with 50mL 1mM chlorauric acid solution be heated to boil after, the citric acid three sodium solution that adds 1～10mL38.8mM rapidly, after the back flow reaction 15min, stop heating, naturally cool to room temperature under stirring, prepare nano-Au solution; Nm of gold in the nano-Au solution solution with the citrate negative ion as protective agent, the about 10～50nm of nanogold particle diameter, the aqueous solution resonance absorbing peak is about 510nm～540nm.
The step of measuring melamine in fluid milk is: liquid milk content of melamine scope: 0-15.2ppm.
(1) takes by weighing liquid milk that 11 parts of 1.6g contain 0ppm, 0.48ppm, 0.95ppm, 1.90ppm, 3.80ppm, 5.70ppm, 7.60ppm, 9.50ppm, 11.4ppm, 13.3ppm, 15.2ppm melamine respectively to the 7ml centrifuge tube, carry out obtaining the liquid milk standard specimen after the described pre-treatment; Get the described nano-Au solution of 0.1mL, the liquid milk standard specimen after the pre-treatment of the different melamine mass ratioes of adding 0.2mL mixes, and measures behind the placement chromogenic reaction 0.5min;
(2) with the color standards series of the milk standard specimen after the chromogenic reaction as visual colorimetry;
Perhaps, adopt ultraviolet-visible spectrophotometer to be determined at 650nm wavelength and 520nm wavelength place absorbance the milk standard specimen after the chromogenic reaction, will be at the ratio A of 650nm and 520nm place absorbance
650/ A
520As horizontal ordinate, the concentration of melamine is as ordinate, and the drawing standard curve also draws the typical curve equation;
(3) take by weighing in liquid milk testing sample 1.6g to the 7ml centrifuge tube, carry out described pre-treatment, get the described nano-Au solution of 0.1mL, add the liquid milk testing sample of 0.2mL pre-treatment, mix, measure behind the placement chromogenic reaction 0.5min; By with the color standards series of comparisons of visual colorimetry, qualitatively judge out whether contain melamine in the liquid milk testing sample;
Perhaps, the liquid milk testing sample after the chromogenic reaction is measured absorbance at 650nm wavelength and 520nm wavelength place, calculate the ratio A of 650nm and 520nm place absorbance
650/ A
520, substitution typical curve equation, quantitative Analysis goes out the amount of melamine in the liquid milk testing sample.
The step of measuring melamine in the milk powder is: milk powder content of melamine scope: 0-79.8ppm
(1) takes by weighing 13 parts of 0.6g and contain the milk powder of 0ppm, 0.84ppm, 1.93ppm, 4.2ppm, 12.6ppm, 21ppm, 29.4ppm, 37.8ppm, 46.2ppm, 54.6ppm, 63ppm, 71.4ppm, 79.8ppm melamine respectively to the 7ml centrifuge tube, add the water-soluble of 2mL and separate, carry out obtaining the milk power solution standard specimen after the described pre-treatment; Get the described nano-Au solution of 0.1mL, the milk power solution standard specimen after the pre-treatment of the different melamine mass ratioes of adding 0.2mL mixes, and measures behind the placement chromogenic reaction 0.5min;
(2) with the color standards series of the milk power solution standard specimen after the chromogenic reaction as visual colorimetry;
Perhaps, adopt ultraviolet-visible spectrophotometer to measure absorbance the milk power solution standard specimen after the chromogenic reaction at 650nm wavelength and 520nm wavelength place, will be at the ratio A of 650nm and 520nm place absorbance
650/ A
520As horizontal ordinate, the concentration of melamine is as ordinate, and the drawing standard curve also draws the typical curve equation;
(3) take by weighing the molten testing sample of milk powder 0.6g to 7ml centrifuge tube, add the water-soluble of 2mL and separate, carry out described pre-treatment, get the described nano-Au solution of 0.1mL, add the liquid milk testing sample of 0.2mL pre-treatment, mix, measure behind the placement chromogenic reaction 0.5min; By with the color standards series of comparisons of visual colorimetry, qualitatively judge out whether contain melamine in the liquid milk testing sample;
Perhaps, the liquid milk testing sample after the chromogenic reaction is measured absorbance at 650nm wavelength and 520nm wavelength place, calculate the ratio A of 650nm and 520nm place absorbance
650/ A
520, substitution typical curve equation, quantitative Analysis goes out the amount of melamine in the milk powder testing sample.
After adding melamine, the color of solution changes immediately, measures behind the placement chromogenic reaction 0.5min; And within long period of time, can not change, in general, at room temperature can place about 1-2 days, can place at least one week at the fridge freshness retaining reefer.
The invention will be further described below in conjunction with embodiment:
The preparation of one .13nm nm of gold
Adopt sodium citrate reduction gold chloride method, the chlorauric acid solution of 50mL 1mM is heated to boils, the trisodium citrate that adds 5mL 38.8mM then rapidly, after the back flow reaction 15min, stop heating, naturally cool to room temperature under stirring, the nm of gold maximum absorption wavelength for preparing gained with this method is 520nm, and the color of solution is a claret.
Two. nm of gold is to the application of melamine detection
Melamine detection in the embodiment 1 nm of gold liquid towards milk
Take by weighing 11 parts of 1.6g and contain 0ppm respectively, 0.48ppm, 0.95ppm, 1.90ppm, 3.80ppm, 5.70ppm, 7.60ppm, 9.50ppm, 11.4ppm, 13.3ppm, 15.2ppm the liquid milk of melamine is to the 7ml centrifuge tube, add 0.72mL trichloroacetic acid (10%) and 1mL chloroform trichloroacetic acid and chloroform, centrifuging after the sonicated (200W sonicated 15 minutes after 13000rpm centrifugal 6 minutes) removes deproteinize and fat, the supernatant of gained transfers to pH 8.0 with the 1M sodium carbonate liquor with its pH, further remove sediment by the method for centrifuging (the centrifugal 1min of 3000rpm) again, get supernatant and carry out the melamine detection by the following method: the nano-Au solution of getting 0.1mL, the liquid milk supernatant that adds the different melamine mass ratioes of 0.2mL, mix, carry out ultraviolet-visible absorption spectroscopy analysis and visual colorimetric analysis after placing chromogenic reaction 0.5min, see Fig. 1, increase along with content of melamine, the absorption peak of nm of gold at the 520nm place is the trend that reduces gradually, peak width increases gradually, and the absorbance at the 650nm place is the trend that increases gradually, at this moment, nm of gold is at the ratio (A of 650nm and 520nm place absorbance
650/ A
520) see Fig. 2 with the melamine concentration relation.Linear equation is Y=0.30166+0.04652X, R=0.99026.Accordingly, the color of nm of gold has redness to gradually change to purple, is changed to blue (see figure 3) by purple again.
Take by weighing 13 parts of 0.6g and contain 0ppm respectively, 0.84ppm, 1.93ppm, 4.2ppm, 12.6ppm, 21ppm, 29.4ppm, 37.8ppm, 46.2ppm, 54.6ppm, 63ppm, 71.4ppm, 79.8ppm the milk powder of melamine is to the 7ml centrifuge tube, water-soluble the separating of secondary that adds 2mL, add 2mL trichloroacetic acid (10%) and 1.2mL chloroform, centrifuging after the sonicated (after the 200W sonicated 15 minutes under the 13000rpm centrifugal 6 minutes) removes deproteinize and fat, the supernatant of gained transfers to pH 7.0 with the 1M sodium carbonate liquor with its pH, further remove sediment by the method for centrifuging (centrifugal 1min under the 3000rpm) again, get supernatant and carry out the melamine detection by the following method: the nano-Au solution of getting 0.1mL, the milk powder supernatant that adds the different melamine mass ratioes of 0.2mL, mix, carry out the ultraviolet-visible absorption spectroscopy analysis respectively after placing chromogenic reaction 0.5min, see Fig. 4, increase along with content of melamine, the absorption peak of nm of gold at the 520nm place is the trend that reduces gradually, peak width increases gradually, and the absorbance at the 650nm place is the trend that increases gradually, at this moment, nm of gold is at the ratio (A of 650nm and 520nm place absorbance
650/ A
520) see Fig. 5 with the melamine concentration relation.Linear equation is Y=0.23647+0.00281X, R=0.99359.Accordingly, the color of nm of gold has redness to gradually change to the purple (see figure 6).
Claims (10)
1. method based on melamine in the nm of gold fast detecting milk sample, it is characterized in that: after milk sample is carried out pre-treatment, be added in the nano-Au solution, adopt visual colorimetry, nm of gold color and color standards series behind the adding sample solution are compared, qualitatively judge in the milk whether contain melamine; Being prepared as of described color standards series: the milk standard specimen that contains the variable concentrations melamine that adopts equal volume through pre-treatment, it is added in the nano-Au solution, contained nm of gold amount unanimity in each sample after the chromogenic reaction, obtains color standards series.
2. method based on melamine in the nm of gold fast detecting milk sample, it is characterized in that: after milk sample is carried out pre-treatment, adopt ultraviolet-visible spectrophotometer to measure absorbance after being added to nano-Au solution, the absorbance of measuring is introduced the content that the typical curve Equation for Calculating obtains melamine in the milk; Described typical curve equation: the milk standard specimen that contains the variable concentrations melamine that adopts equal volume through pre-treatment, it is added in the nano-Au solution, contained nm of gold amount unanimity in each sample, after the chromogenic reaction, adopt the ultraviolet-visible spectrophotometer working sample in 650nm wavelength and 520nm wavelength place absorbance, with its ratio A in 650nm and 520nm place absorbance
650/ A
520As horizontal ordinate, the concentration of melamine is as ordinate, and the drawing standard curve also draws the typical curve equation.
3. the method based on melamine in the nm of gold fast detecting milk sample according to claim 2, it is characterized in that: the concentration content range of the melamine that can measure is 0～15.2ppm for liquid milk, is 0～79.8ppm for milk powder; The making scope of typical curve is 0～15.2ppm according to liquid milk, and milk powder is 0～79.8ppm, gets the point of some variable concentrations, measures absorbance at 650nm wavelength and 520nm wavelength place, will be at the ratio A of 650nm and 520nm place absorbance
650/ A
520As horizontal ordinate, the concentration of melamine is as ordinate, and the drawing standard curve also draws the typical curve equation.
4. according to claim 1,2 or 3 described methods based on melamine in the nm of gold fast detecting milk sample, it is characterized in that described milk sample carries out pre-treatment and is: in milk, add trichloroacetic acid and chloroform, for liquid milk and milk powder, adding 0.45mL concentration in every gram liquid milk is 10wt% trichloroacetic acid and 0.625mL chloroform; Adding 3.33mL concentration in every gram milk powder is 10wt% trichloroacetic acid and 2mL chloroform, according to centrifugal 6 minutes of 13000rpm after the 200W sonicated 15 minutes, remove deproteinize and fat, the supernatant of gained transfers to pH 7.0-8.0 with the 1M sodium carbonate liquor with its pH, pass through the centrifugal 1min of 3000rpm again, further remove sediment, get the milk sample after supernatant is pre-treatment; The pre-treatment of described milk standard specimen is identical with the milk sample pre-treatment.
5. the method based on melamine in the nm of gold fast detecting milk sample according to claim 4 is characterized in that: when the detection thing is milk powder, milk powder is dissolved in the water, handles according to the step of described milk sample pre-treatment.
6. the method based on melamine in the nm of gold fast detecting milk sample according to claim 4 is characterized in that: the nano-Au solution that the milk sample after the 0.2mL pre-treatment or standard specimen is added to 0.1mL; Being prepared as of described nano-Au solution: adopt sodium citrate reduction gold chloride method, with the chlorauric acid solution of 50mL 1mM be heated to boil after, add 1～10mL 38.8mM citric acid three sodium solution rapidly, after the back flow reaction 15min, stop heating, naturally cool to room temperature under stirring, prepare nano-Au solution.
7. the method based on melamine in the nm of gold fast detecting milk sample according to claim 6; it is characterized in that: the nm of gold in the described nano-Au solution with the citrate negative ion as protective agent; about 10～the 50nm of nanogold particle diameter, the aqueous solution resonance absorbing peak is about 518nm～540nm.
8. according to claim 1,2 or 3 described methods, it is characterized in that: measure behind the chromogenic reaction 0.5min based on melamine in the nm of gold fast detecting milk sample.
9. the method based on melamine in the nm of gold fast detecting milk sample according to claim 8 is characterized in that: the step that described method is measured melamine in fluid milk is:
(1) takes by weighing liquid milk that 11 parts of 1.6g contain 0ppm, 0.48ppm, 0.95ppm, 1.90ppm, 3.80ppm, 5.70ppm, 7.60ppm, 9.50ppm, 11.4ppm, 13.3ppm, 15.2ppm melamine respectively to the 7ml centrifuge tube, carry out obtaining the liquid milk standard specimen after the described pre-treatment; Get the described nano-Au solution of 0.1mL, the liquid milk standard specimen after the pre-treatment of the different melamine mass ratioes of adding 0.2mL mixes, and measures behind the placement chromogenic reaction 0.5min;
(2) with the color standards series of the milk standard specimen after the chromogenic reaction as visual colorimetry;
Perhaps, adopt ultraviolet-visible spectrophotometer to measure it milk standard specimen after chromogenic reaction in 650nm wavelength and 520nm wavelength place absorbance, will be at the ratio A of 650nm and 520nm place absorbance
650/ A
520As horizontal ordinate, the concentration of melamine is as ordinate, and the drawing standard curve also draws the typical curve equation;
(3) take by weighing in liquid milk testing sample 1.6g to the 7ml centrifuge tube, carry out described pre-treatment, get the described nano-Au solution of 0.1mL, add the liquid milk testing sample of 0.2mL pre-treatment, mix, measure behind the placement chromogenic reaction 0.5min; By with the color standards series of comparisons of visual colorimetry, qualitatively judge out whether contain melamine in the liquid milk testing sample, detect melamine in fluid milk content range: 0～15.2ppm;
Perhaps, the liquid milk testing sample after the chromogenic reaction is measured absorbance at 650nm wavelength and 520nm wavelength place, calculate the ratio A of 650nm and 520nm place absorbance
650/ A
520, substitution typical curve equation, quantitative Analysis goes out the amount of melamine in the liquid milk testing sample.
10. the method based on melamine in the nm of gold fast detecting milk sample according to claim 9 is characterized in that: the step that described method is measured melamine in the milk powder is:
(1) takes by weighing 13 parts of 0.6g and contain the milk powder of 0ppm, 0.84ppm, 1.93ppm, 4.2ppm, 12.6ppm, 21ppm, 29.4ppm, 37.8ppm, 46.2ppm, 54.6ppm, 63ppm, 71.4ppm, 79.8ppm melamine respectively to the 7ml centrifuge tube, add the water-soluble of 2mL and separate, carry out obtaining the milk power solution standard specimen after the described pre-treatment; Get the described nano-Au solution of 0.1mL, the milk power solution standard specimen after the pre-treatment of the different melamine mass ratioes of adding 0.2mL mixes, and measures behind the placement chromogenic reaction 0.5min;
(2) with the color standards series of the milk power solution standard specimen after the chromogenic reaction as visual colorimetry;
Perhaps, adopt ultraviolet-visible spectrophotometer to be determined at 650nm and 520nm place absorbance the milk power solution standard specimen after the chromogenic reaction, will be at the ratio A of 650nm and 520nm place absorbance
650/ A
520As horizontal ordinate, the concentration of melamine is as ordinate, and the drawing standard curve also draws the typical curve equation;
(3) take by weighing milk powder testing sample 0.6g to 7ml centrifuge tube, add the water-soluble of 2mL and separate, carry out described pre-treatment, get the described nano-Au solution of 0.1mL, add the milk powder testing sample of 0.2mL pre-treatment, mix, measure behind the placement chromogenic reaction 0.5min; By with the color standards series of comparisons of visual colorimetry, qualitatively judge out whether contain melamine in the milk powder testing sample;
Perhaps, milk powder testing sample after the chromogenic reaction is measured absorbance at 650nm wavelength and 520nm wavelength place, calculate the ratio A650/A520 of 650nm and 520nm place absorbance, substitution typical curve equation, quantitative Analysis goes out the amount of melamine in the liquid milk testing sample, detects content of melamine scope: 0～79.8ppm in the milk powder.
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