CN109060745B - Melamine detection method - Google Patents

Melamine detection method Download PDF

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CN109060745B
CN109060745B CN201810952668.4A CN201810952668A CN109060745B CN 109060745 B CN109060745 B CN 109060745B CN 201810952668 A CN201810952668 A CN 201810952668A CN 109060745 B CN109060745 B CN 109060745B
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melamine
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gold nanocluster
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CN109060745A (en
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张现峰
芦静波
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Jiangsu Quanzheng Inspection & Testing Co ltd
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Bengbu College
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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
    • G01N21/62—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
    • G01N21/63—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light optically excited
    • G01N21/64—Fluorescence; Phosphorescence
    • G01N21/6428—Measuring fluorescence of fluorescent products of reactions or of fluorochrome labelled reactive substances, e.g. measuring quenching effects, using measuring "optrodes"
    • G01N21/643—Measuring fluorescence of fluorescent products of reactions or of fluorochrome labelled reactive substances, e.g. measuring quenching effects, using measuring "optrodes" non-biological material
    • 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
    • G01N21/62—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
    • G01N21/63—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light optically excited
    • G01N21/64—Fluorescence; Phosphorescence
    • G01N21/6428—Measuring fluorescence of fluorescent products of reactions or of fluorochrome labelled reactive substances, e.g. measuring quenching effects, using measuring "optrodes"
    • G01N2021/6432—Quenching

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Abstract

The invention discloses a melamine detection method, which takes Bovine Serum Albumin (BSA) as a reducing agent and a stabilizing agent to reduce HAuCl4The gold nanocluster BSA-AuNCs with red fluorescence are synthesized in an alkaline aqueous solution, a detection system containing known melamine concentration is constructed, a fluorescence spectrometer is adopted to determine the fluorescence emission intensity at 635nm and make a standard curve, then a pre-treated object to be detected is added into a solution of the mercaptophenylboronic acid modified gold nanocluster, finally the fluorescence intensity at 635nm is determined, the melamine concentration in the object to be detected is obtained by contrasting the standard curve, the accuracy is high, the processing is simple, the whole process is simple and convenient to operate, the response is quick, and the detection requirement of people for quickly screening melamine residue in a milk product at present can be met.

Description

Melamine detection method
Technical Field
The invention belongs to the technical field of food quality detection, and particularly relates to a melamine detection method.
Background
Melamine is commonly called melamine and protamine, is a triazine nitrogen-containing heterocyclic organic compound and is used as a chemical raw material. It is a white monoclinic crystal, almost odorless, slightly soluble in water (3.1 g/L at room temperature), soluble in methanol, formaldehyde, acetic acid, hot ethylene glycol, glycerol, pyridine, etc., and insoluble in acetone and ethers. Non-flammable and stable in property at normal temperature. Aqueous solutions are weakly alkaline (pH = 8) and form melamine salts with hydrochloric acid, sulfuric acid, nitric acid, acetic acid, oxalic acid, and the like. It contains nitrogen up to 66.6%, is a white crystalline powder, has no odor and taste, is not easily found after being mixed, is harmful to human body, and is not applicable to food processing or food additives, and if 0.1g of melamine is added to 100g of milk, the false content of protein can be increased by 0.4%. Under neutral or slightly alkaline condition, the formaldehyde and the formaldehyde are condensed to form various methylol melamines, but the methylol derivatives are subjected to polycondensation reaction in slightly acidic condition (pH value is 5.5-6.5) to form resin products. When the cyanuric acid is hydrolyzed by strong acid or strong alkali aqueous solution, the amido is gradually replaced by hydroxyl, ammeline is firstly generated, ammelide is further generated by hydrolysis, and cyanuric acid is finally generated. Wherein, the melamine and the cyanuric acid can form a water-insoluble network associated macromolecular compound through the intermolecular hydrogen bond interaction, thereby causing serious kidney stones.
The food quality supervision and inspection center of China indicates that melamine belongs to chemical raw materials and is not allowed to be added into food in 2008, 9, 13 days, so that standard limits such as pesticide residues are not set temporarily. And in 8 days after 10 months, the ministry of health, the ministry of industry and informatization, the ministry of agriculture, the State administration of Industrial and commercial administration and the State administration of quality supervision, inspection and quarantine jointly issue bulletins, and the temporary management value of the melamine in the milk and the dairy products is formulated:
the limit value of melamine in the infant formula milk powder is 1 mg/kg, and products higher than 1 mg/kg cannot be sold uniformly. The limit value of melamine in liquid milk (including raw milk), milk powder and other formula milk powder is 2.5mg/kg, and products higher than 2.5mg/kg cannot be sold uniformly. The limit value of melamine in other food containing more than 15% of milk is 2.5mg/kg, and products higher than 2.5mg/kg cannot be sold uniformly.
7/5/2012, the international food code committee of the united nations who is responsible for establishing food safety standards set a new standard for the melamine content in milk, and later, the melamine content in each kilogram of liquid milk must not exceed 0.15 mg. The international food code committee states that new standards for melamine content will help governments better protect consumer rights and health.
At present, the detection of melamine mainly comprises high performance liquid chromatography, liquid chromatography-mass spectrometry and the like. In addition, enzyme-linked immunosorbent assay, capillary electrochromatography, mass spectrometry and infrared absorption spectroscopy are reported in documents, and the methods generally need complex sample pretreatment, are expensive in instrument price, are complex to operate, have high detection cost, can be operated by professionals, and cannot completely meet the detection requirement of rapidly screening melamine residue in milk. Therefore, it is necessary to provide a melamine detection method which is easy to operate, has a rapid response and has a low detection limit.
Disclosure of Invention
The invention aims to make up for the defects of the prior art and provides a melamine detection method.
The invention is realized by the following technical scheme:
a method for detecting melamine comprises reducing HAuCl with bovine serum albumin BSA as reducing agent and stabilizer4The gold nanocluster modified by the mercapto phenylboronic acid is prepared, a detection system containing the known melamine concentration is constructed, the fluorescence emission intensity of the gold nanocluster at 635nm is measured by a fluorescence spectrometer, a standard curve is made, the pretreated object to be measured is added into the mercapto phenylboronic acid modified gold nanocluster solution, the fluorescence intensity of the pretreated object to be measured at 635nm is measured, and the melamine concentration of the object to be measured is obtained by contrasting the standard curve.
The preparation method of the gold nanocluster modified by mercaptophenylboronic acid comprises the following steps:
(1) 10mL of 1mM HAuCl4Uniformly mixing the solution with 10mL of 50mg/mL BSA solution, adding 2mL of 0.9M NaOH solution, stirring again, uniformly mixing, placing the mixed solution in an ultrasonic cleaner, performing ultrasonic treatment for 55-65min, then placing the mixed solution in a 300W microwave oven, and performing microwave radiation for 35-45s to obtain a BSA-AuNCs gold nanocluster solution;
(2) adding 20 mu L of 5mmol/L mercaptophenylboronic acid solution into the product obtained in the step 1, placing the solution in a 50mL round-bottom flask, adding magnetons, and placing the flask on a magnetic stirrer to carry out magnetic stirring for 4-5 hours;
(3) and (3) placing 10mL of the product prepared in the step (2) into a dialysis bag, clamping clamps at two ends, placing into a beaker, adding pure water into the beaker, immersing the beaker in the dialysis bag, and dialyzing on a magnetic stirrer for 20-24 hours to obtain the gold nanocluster modified by the mercaptophenylboronic acid.
The melamine concentration detection system is constructed by preparing melamine standard solutions with different concentrations, adding the melamine standard solutions into a mercaptophenylboronic acid modified gold nanocluster solution, standing for 25-35min, measuring the fluorescence intensity of the solution, and drawing a standard curve of the fluorescence intensity F0-F and the melamine concentration, wherein F0 represents the fluorescence intensity of the gold nanoclusters at 635nm when melamine is not added, and F represents the fluorescence intensity of the gold nanoclusters at 635nm when melamine is added.
The method for detecting the melamine concentration in the object to be detected comprises the steps of pretreating different types of milk products, adding the milk products into a mercaptophenylboronic acid modified gold nanocluster solution, standing for 25-35min, measuring fluorescence intensity, and comparing with a standard curve to obtain the melamine content in the sample.
The pretreatment method of the object to be detected comprises the following steps:
(1) sampling a milk powder sample by 5g and a liquid milk product by 20g, accurately adding the milk powder sample into 50mL of 10g/L trichloroacetic acid solution, accurately adding 5mL of lead acetate solution to separate protein, shaking up the test solution, ultrasonically oscillating for 25-35min, standing for 5-6min, taking 28-32mL of upper-layer extracting solution, transferring the upper-layer extracting solution to a centrifuge tube, and centrifuging for 5-6min on a 10000r/min centrifuge;
(2) respectively activating the mixed type cation exchange solid-phase extraction column by using 3mL of methanol and 3mL of water, accurately transferring 10mL of centrifugate to the column in a grading manner, enabling the centrifugate to pass through the column at a column passing speed of 0.4-0.6mL/min, washing the mixed type cation exchange solid-phase extraction column by using 3mL of water and 3mL of methanol, eluting the column by using 3mL of 5% ammonia water after being pumped to be nearly dry, drying the eluent by using 45-degree nitrogen, adding 10mL of deionized water into residues, oscillating for 1-2min, and passing through a 0.45-micrometer filter membrane to obtain a sample of an object to be detected.
The invention has the advantages that:
the invention takes bovine serum albumin BSA as a reducing agent and a stabilizing agent to reduce HAuCl4Gold nanocluster BSA-AuNCs with red fluorescence are synthesized in an alkaline aqueous solution, wherein the particles can be driven to vibrate in a reciprocating manner under the action of ultrasound, the dispersibility of a product is enhanced, the agglomeration phenomenon of nanoparticles is effectively prevented, microwave radiation is assisted at the same time, heat is transferred from the inside to the outside of the first heat, compared with the traditional heating, the gold nanocluster BSA-AuNCs are quicker and more uniform, the heating efficiency is higher, the preparation time is shortened, the energy consumption is reduced, multiple hydrogen bonds are formed between phenylboronic acid and melamine, the distance of the gold nanoclusters is reduced, different degrees of fluorescence quenching are caused, the fluorescence intensity is different, and after the color influence of impurities such as various proteins in a milk product is removed through previous treatment, sulfydryl is addedIn the gold nanocluster solution modified by phenylboronic acid, the fluorescence intensity is measured and compared, the accuracy is high, the treatment is simple, the whole process is simple and convenient to operate, the response is quick, and the detection requirement of people for quickly screening melamine residues in milk products at present can be met.
Drawings
FIG. 1 is a schematic diagram showing the principle of detecting melamine by using gold nanoclusters modified by mercaptophenylboronic acid.
FIG. 2 shows fluorescence spectra of gold nanoclusters in solution with different concentrations of melamine.
FIG. 3 shows the relationship between the concentration of melamine and the difference F0-F in fluorescence intensity.
Detailed Description
The technical scheme of the invention is further explained by combining the specific examples as follows:
10mL of 1mM HAuCl4Uniformly mixing the solution with 10mL of 50mg/mL BSA solution, adding 2mL of 0.9M NaOH solution, stirring again, uniformly mixing, placing the mixed solution in an ultrasonic cleaner for ultrasonic treatment for 60min, then placing the mixed solution in a 280W microwave oven, and performing microwave radiation for 40s to obtain the BSA-AuNCs gold nanocluster solution, wherein the solution is bright brown in color, and the solution is placed in a dark box type ultraviolet analyzer to emit red fluorescence.
To the above product was added 20. mu.L of a 5mmol/L mercaptophenylboronic acid solution, placed in a 50mL round bottom flask, added magnetons, and placed on a magnetic stirrer to magnetically stir for 4 h.
And (3) putting 10mL of the gold nanocluster modified by the mercaptophenylboronic acid into a dialysis bag, putting the dialysis bag into a beaker filled with 2000mL of pure water, and dialyzing for 24h to obtain the gold nanocluster modified by the mercaptophenylboronic acid.
Adding melamine standard solutions (0, 0.05, 0.1, 0.2, 0.4, 0.6, 0.8, 1.0, 2.0, 4.0, 6.0 and 10 mu M) with different concentrations into the gold nanocluster solution modified by the mercaptophenylboronic acid respectively, reacting for 30min, and causing the distance between gold nanocluster particles to decrease and causing fluorescence quenching with different degrees due to multiple hydrogen bonds formed between the phenylboronic acid and the melamine as shown in figure 1, and respectively measuring fluorescence spectra of the gold nanocluster solutions, wherein as shown in figure 2, it can be obviously seen that the fluorescence intensity of the gold nanocluster solution decreases with the increase of the melamine concentration, as shown in figure 3, a standard curve of fluorescence intensity F0-F and the melamine concentration is drawn, wherein F0 represents the fluorescence intensity of the gold nanocluster at 635nm when the melamine is not added, F represents the fluorescence intensity of the gold nanocluster at 635nm when the melamine is added, and the melamine concentration is in the range of 0-1.0 mu M, the standard curve is fitted to obtain: y =12.95 + 164.70x (R2 = 0.982), and the minimum detection limit of the standard curve is found to be 16.7nM based on the ratio of the standard deviation to the slope of the standard curve.
Different dairy products (milk powder, pure milk, yoghurt) were pretreated: sampling a milk powder sample by 5g, accurately adding a liquid milk product by 20g into 50mL of 10g/L trichloroacetic acid solution, accurately adding 5mL of lead acetate solution to separate protein, shaking up a test solution, ultrasonically oscillating for 30min, standing for 5min, taking about 30mL of upper-layer extracting solution, transferring the upper-layer extracting solution to a centrifuge tube, centrifuging for 5min on a 10000r/min centrifuge, adding melamine into the centrifugate to enable the concentration of the melamine to be 0.4 mu M, and marking as a labeling solution, wherein the pretreatment has the function of removing the influence of impurities such as various proteins in milk.
Respectively activating the mixed type cation exchange solid-phase extraction column by using 3mL of methanol and 3mL of water, accurately transferring 10mL of added standard solution to the column in a grading manner, enabling the mixed type cation exchange solid-phase extraction column to pass through the column at a speed of about 0.5mL/min, washing the mixed type cation exchange solid-phase extraction column by using 3mL of water and 3mL of methanol, eluting the mixed type cation exchange solid-phase extraction column by using 3mL of 5% ammonia water after being pumped to be nearly dry, blowing the eluent by using 45-degree nitrogen for drying, adding 10mL of deionized water into residues, oscillating for 1min, and passing through a 0.45.
And (3) measuring the content of melamine in the eluent by using a fluorescence spectrometry, adding the eluent into a gold nanocluster solution modified by mercaptophenylboronic acid, reacting for 30min, measuring the fluorescence intensity, comparing with a standard curve to obtain the content of melamine in milk powder, pure milk and yoghourt samples, and calculating the recovery rates of 114%, 108% and 92% respectively.

Claims (4)

1. The melamine detection method is characterized in that bovine serum albumin BSA is used as a reducing agent and a stabilizing agent to reduce HAuCl4Preparation to obtain BSA-AuNCs gold nanocluster, modifying the BSA-AuNCs gold nanocluster by utilizing a mercaptophenylboronic acid solution to prepare the mercaptophenylboronic acid modified gold nanocluster, determining the fluorescence emission intensity at 635nm by adopting a fluorescence spectrometer and making a standard curve by constructing a detection system containing known melamine concentration, adding a pre-treated object to be detected into the mercaptophenylboronic acid modified gold nanocluster solution, determining the fluorescence intensity at 635nm, and obtaining the concentration of melamine in the object to be detected by contrasting the standard curve;
the preparation method of the gold nanocluster modified by mercaptophenylboronic acid comprises the following steps:
(1) 10mL of 1mM HAuCl4Uniformly mixing the solution with 10mL of 50mg/mL BSA solution, adding 2mL of 0.9M NaOH solution, stirring again, uniformly mixing, placing the mixed solution in an ultrasonic cleaner, performing ultrasonic treatment for 55-65min, then placing the mixed solution in a 300W microwave oven, and performing microwave radiation for 35-45s to obtain a BSA-AuNCs gold nanocluster solution;
(2) adding 20 mu L of 5mmol/L mercaptophenylboronic acid solution into the prepared product in the step (1), placing the mixture into a 50mL round-bottom flask, adding magnetons, and placing the mixture on a magnetic stirrer to carry out magnetic stirring for 4-5 hours;
(3) and (3) placing 10mL of the product prepared in the step (2) into a dialysis bag, clamping clamps at two ends, placing the dialysis bag into a beaker, adding pure water into the beaker, immersing the beaker in the dialysis bag, and then placing the dialysis bag on a magnetic stirrer for dialysis for 20-24 hours to obtain the gold nanocluster modified by the mercaptophenylboronic acid.
2. The method for detecting melamine as claimed in claim 1, wherein the detection system containing known melamine concentration is constructed by preparing melamine standard solutions with different concentrations, adding the melamine standard solutions into the mercaptophenylboronic acid modified gold nanocluster solution, standing for 25-35min, measuring the fluorescence intensity, and drawing a standard curve of fluorescence intensity F0-F and melamine concentration, wherein F0 represents the fluorescence intensity of the gold nanoclusters at 635nm when no melamine is added, and F represents the fluorescence intensity of the gold nanoclusters at 635nm when melamine is added.
3. The method for detecting melamine according to claim 1, wherein the method for detecting the melamine concentration in the object to be detected comprises the steps of pretreating different types of milk products, adding the milk products into the gold nanocluster solution modified by the mercaptophenylboronic acid, standing for 25-35min, measuring the fluorescence intensity, and comparing the fluorescence intensity with a standard curve to obtain the melamine content in the sample.
4. The melamine detection method according to claim 3, wherein the pretreatment method of the object to be measured comprises the steps of:
(1) sampling a milk powder sample by 5g and a liquid milk product by 20g, accurately adding the milk powder sample into 50mL of 10g/L trichloroacetic acid solution, accurately adding 5mL of lead acetate solution to separate protein, shaking up the sample solution, ultrasonically oscillating for 25-35min, standing for 5-6min, taking 28-32mL of upper-layer extracting solution, transferring the upper-layer extracting solution to a centrifuge tube, and centrifuging for 5-6min on a 10000r/min centrifuge;
(2) respectively activating the mixed type cation exchange solid-phase extraction column by using 3mL of methanol and 3mL of water, accurately transferring 10mL of centrifugate to the column in a grading manner, enabling the centrifugate to pass through the column at a column passing speed of 0.4-0.6mL/min, washing the mixed type cation exchange solid-phase extraction column by using 3mL of water and 3mL of methanol, eluting the column by using 3mL of 5% ammonia water methanol solution after being pumped to be nearly dry, drying the eluent by using 45-degree nitrogen, adding 10mL of deionized water into residues, shaking for 1-2min, and passing the residues through a 0.45-micrometer filter membrane to obtain a sample of an object.
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CN115572597A (en) * 2022-09-30 2023-01-06 青岛大学 Thiobabituric acid-gold nanocluster and preparation method and application thereof

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CN103901008A (en) * 2014-04-18 2014-07-02 吉林大学 Detection on melamine in hen eggs through inner filtration effect of fluorescence
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