CN108918434A - Application of the mantoquita in detection melamine and/or cyanuric acid - Google Patents
Application of the mantoquita in detection melamine and/or cyanuric acid Download PDFInfo
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- CN108918434A CN108918434A CN201810286323.XA CN201810286323A CN108918434A CN 108918434 A CN108918434 A CN 108918434A CN 201810286323 A CN201810286323 A CN 201810286323A CN 108918434 A CN108918434 A CN 108918434A
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Abstract
The invention discloses application of the mantoquita in detection melamine and/or cyanuric acid.Inventor's discovery：Copper salt solution generates copper oxide nanometer particle in no cyanuric acid under certain condition, and solution colour is caused to change；Copper salt solution generates various concentration copper oxide nanometer particle under certain condition or does not generate copper oxide nanometer particle, different colors is presented with the difference of cyanuric acid concentration in solution colour variation in the presence of the cyanuric acid of various concentration.Using color variation can qualitative or half-quantitative detection melamine or cyanuric acid content, can be with the content of quantitative detection melamine or cyanuric acid using UV-visible spectrometer.In turn, the present invention also provides a kind of methods of detection melamine and/or cyanuric acid.This method is simple, cheaply, quickly, and sensitive, specific height, the quick detection suitable for melamine in actual sample or cyanuric acid.
Description
Technical field
The present invention relates to medicine, food or environmental tests and determination techniques field, in particular to mantoquita is in detection melamine
Application in amine and/or cyanuric acid.
Background technique
Melamine (English:Melamine, chemical formula:C3N3(NH2)3), it is commonly called as melamine, extract of protein, IUPAC is named as "
1,3,5-triazines -2,4,6- triamine ", it is a kind of triazines nitrogen heterocyclic ring organic compound, is used as industrial chemicals.Due to trimerization
The nitrogen content of cyanamide can reach 66%, be often added in food or feed by illegal businessman, contain to raise the protein of product
Amount, brings bad influence to consumer.Therefore, China national food quality supervision inspection center referred on September 13rd, 2008
Out, melamine belongs to industrial chemicals, is not allow to be added in food.
The method of detection melamine has gas-chromatography-mass spectrography, ultra performance liquid chromatography-electron spray series connection matter at present
Spectrometry, reversed-phased high performace liquid chromatographic, high performance liquid chromatography-diode array, high performance liquid chromatography, high-efficient liquid phase color
Spectrum-quadrupole rod mass spectrometry, Solid Phase Extraction and high performance liquid chromatography combination, liquid chromatography tandem mass spectrometry one, enzyme assay etc.
Method.These testing costs are high, and test speed is slower.
Summary of the invention
The primary purpose of the present invention is that the shortcomings that overcoming the prior art and deficiency, provide mantoquita in detection melamine
And/or the application in cyanuric acid.
Another object of the present invention is to provide a kind of methods of detection melamine and/or cyanuric acid.
The purpose of the invention is achieved by the following technical solution：Mantoquita is in detection melamine and/or cyanuric acid
Using.The technical solution is found based on inventor：Copper salt solution generates under certain condition in no cyanuric acid
Copper oxide nanometer particle causes solution colour to change；Copper salt solution is in the presence of the cyanuric acid of various concentration, in certain condition
Lower production various concentration copper oxide nanometer particle does not generate copper oxide nanometer particle, and solution colour changes with cyanuric acid concentration
Difference and different colors is presented.It can qualitative or half-quantitative detection melamine or cyanuric acid using the variation of color
Content, can be with the content of quantitative detection melamine or cyanuric acid using UV-visible spectrometer.
The mantoquita refers to soluble copper salt, preferably one of copper sulphate, copper acetate, copper chloride and copper nitrate
Or at least two.
Application of the mantoquita in detection melamine and/or cyanuric acid, including to melamine and/or cyanuric acid into
Row qualitative detection and quantitative detection.
When carrying out the qualitative detection, include the following steps：
(1-1) when only whether detection sample to be tested contains cyanuric acid, steps are as follows：
(A) sample to be tested is configured to the solution of various concentration, copper salt solution is subsequently added into, obtains reaction system, one
A period of time is reacted under the conditions of fixed pH and temperature；
(B) when brown or brown color occurs in the solution of all various concentrations of preparation, tentatively judge testing sample solution
In do not contain cyanuric acid；When there are concentration solution keep present light blue or blue-green when, show that sample to be tested is molten
Contain cyanuric acid in liquid；
(1-2) when only whether detection sample to be tested contains cyanuric acid and melamine, steps are as follows：
1. the processing of sample to be tested：
(A) a part of sample to be tested is taken, the testing sample solution of various concentration is configured to；
(B) a part of testing sample solution and strong acid are mixed, reaction is hydrolyzed；Then highly basic reaction is added, obtains
Treatment fluid；Treatment fluid is carried out to the dilution of certain gradient, is the treatment fluid of various concentration；
2. detecting：
(A) it is separately added into copper salt solution in the testing sample solution of various concentration, obtains reaction system, in certain pH
It is reacted for a period of time under the conditions of temperature, obtains a series of reaction solution A；
(B) it is separately added into copper salt solution in the treatment fluid of various concentration, obtains reaction system, in certain pH and temperature
Under the conditions of react a period of time, obtain a series of reaction solution B；
3. the judgement of result：
(A) when brown or brown color occur in all reaction solution A and all reaction solution B, tentatively judge sample to be tested
Cyanuric acid and melamine are not contained in solution；
(B) when brown or brown color occur in all reaction solution A, in a series of reaction solution B there are concentration
When blue-green or blue-green is presented in reaction solution B, melamine is contained only in preliminary judgement sample solution；
(C) when there are the reaction solution A and the reaction solution B of concentration that has of concentration blue-green or blue-green is presented when, feelings
Condition is specific as follows：
(a) when the light absorption value of reaction solution A and reaction solution B at 400nm of the test substance of homogenous quantities containing phase is identical, tentatively sentence
Disconnected sample to be tested is free of melamine containing only cyanuric acid；
(b) light absorption value as the reaction solution A and reaction solution B of the test substance of homogenous quantities containing phase at 400nm is reaction solution A >
Reaction solution B tentatively judges in sample to be tested containing melamine and cyanuric acid.
In step (1-1) (A)：
The solvent of the preparation is water or buffer solution.
The buffer solution is preferably citric acid-disodium hydrogen phosphate buffer, ammonia-ammonium chloride buffer, acetic acid-acetic acid
Sodium buffer, phosphate buffer solution, Tris-HCl buffer solution or HEPES buffer solution.
The concentration of the buffer solution is preferably 0.1mM~1M, can be 0.1mM, 0.5mM, 1mM, 5mM, 10mM,
100mM,1000mM；More preferably 10~100mM.
Concentration of the mantoquita in the reaction system be 0.1mM~10mM, can be 0.1mM, 0.5mM,
0.75mM,1mM,5mM,10mM；Preferably 0.5~1mM；More preferably 0.75mM.This is 1.5 to convert according to embodiment
× 10 ÷ 20=0.75mM
The pH is 3~10, can be 3,4,5,6,7,8,9,10；Preferably 6~8.
The temperature is 40~100 DEG C, can be 40 DEG C, 50 DEG C, 60 DEG C, 70 DEG C, 80 DEG C, 90 DEG C, 100 DEG C；It is preferred that
It is 60~100 DEG C.
The time is 1min~2h, can be 1min, 10min, 30min, 50min, 1h, 1.5h, 2h；Preferably
5min~1h.
Step (1-2) is 1. in (A)：
The solvent of the preparation is water or buffer solution.
The buffer solution is preferably citric acid-disodium hydrogen phosphate buffer, ammonia-ammonium chloride buffer, acetic acid-acetic acid
Sodium buffer, phosphate buffer solution, Tris-HCl buffer solution or HEPES buffer solution.
The concentration of the buffer solution is preferably 10~100mM.
Step (1-2) is 1. in (B)：
The strong acid is preferably one of hydrochloric acid, sulfuric acid, phosphoric acid and nitric acid or at least two.
The concentration of the strong acid is preferably 10M.
The dosage of the strong acid presses its concentration in hydrolysis reaction system preferably as 0.8~1.2M calculating；It is preferred that
For by its concentration in hydrolysis reaction system be 1M calculate.
The condition of the hydrolysis is preferably 90~100 DEG C of heating 30min~2h；Preferably 100 DEG C heating
60min。
The highly basic is preferably one or both of sodium hydroxide and potassium hydroxide.
The dosage of the highly basic preferably presses highly basic hydroxyl molal quantity：Hydrogen radical mole number of ions=1 of strong acid：1 meter
It calculates.
Solvent used in the dilution is water or buffer solution.
The buffer solution is preferably citric acid-disodium hydrogen phosphate buffer, ammonia-ammonium chloride buffer, acetic acid-acetic acid
Sodium buffer, phosphate buffer solution, Tris-HCl buffer solution or HEPES buffer solution.
The concentration of the buffer solution is preferably 0.1mM~1M, can be 0.1mM, 0.5mM, 1mM, 5mM, 10mM,
100mM,1000mM；More preferably 10~100mM.
Step (1-2) 2. in：
Concentration of the mantoquita in the reaction system be 0.1mM~10mM, can be 0.1mM, 0.5mM,
0.75mM,1mM,5mM,10mM；Preferably 0.5~1mM；More preferably 0.75mM.
The pH is 3~10, can be 3,4,5,6,7,8,9,10；Preferably 6~8.
The temperature is 40~100 DEG C, can be 40 DEG C, 50 DEG C, 60 DEG C, 70 DEG C, 80 DEG C, 90 DEG C, 100 DEG C；It is preferred that
It is 60~100 DEG C.
The time is 1min~2h, can be 1min, 10min, 30min, 50min, 1h, 1.5h, 2h；Preferably
5min~1h.
When carrying out the quantitative detection, include the following steps：
(2-1) when only detecting the content of cyanuric acid in sample to be tested, steps are as follows：
(A) the cyanuric acid standard solution for preparing various concentration, is added copper salt solution, reaction system is obtained, certain
A period of time is reacted under the conditions of pH and temperature, the measurement of light absorption value is carried out at 400nm, draws standard curve；
(B) copper salt solution is added in testing sample solution, obtains reaction system, it is anti-under the conditions of certain pH and temperature
It should a period of time；Then the measurement of light absorption value is carried out at 400nm, establishing criteria curve obtains cyanuric acid in sample to be tested
Content；
(2-2) when containing only melamine in sample to be tested, the step of melamine, is as follows in detection sample to be tested：
(A) melamine of various concentration and strong acid are mixed, reaction is hydrolyzed；Then highly basic reaction is added, obtains
Melamine treatment fluid；Copper salt solution is added in melamine treatment fluid, obtains reaction system, in certain pH and temperature strip
A period of time is reacted under part；Then the measurement that light absorption value is carried out at 400nm, draws standard curve；
(B) testing sample solution and strong acid are mixed, reaction is hydrolyzed；Then highly basic reaction is added, obtains to test sample
Product treatment fluid；Copper salt solution is added in sample to be tested treatment fluid, obtains reaction system, it is anti-under the conditions of certain pH and temperature
It should a period of time；Then the measurement of light absorption value is carried out at 400nm, establishing criteria curve obtains melamine in sample to be tested
Content；
(2-3) detects melamine and trimerization in sample to be tested when sample to be tested contains melamine and cyanuric acid
The step of cyanic acid, is as follows：
(A) according to step (2-1), the content of cyanuric acid is obtained；
(B) according to step (2-2), the total content of cyanuric acid and melamine is obtained；
(C) total content-cyanuric acid content of content=cyanuric acid of melamine and melamine.
In step (2-1) (A)：
The solvent of the preparation is water or buffer solution.
The buffer solution is preferably citric acid-disodium hydrogen phosphate buffer, ammonia-ammonium chloride buffer, acetic acid-acetic acid
Sodium buffer, phosphate buffer solution, Tris-HCl buffer solution or HEPES buffer solution.
The concentration of the buffer solution is preferably 0.1mM~1M, can be 0.1mM, 0.5mM, 1mM, 5mM, 10mM,
100mM,1000mM；More preferably 10~100mM.
In step (2-1) (B)：
When the sample to be tested need to be added solvent and be dissolved and be diluted, solvent is water or buffer solution.
The buffer solution is preferably citric acid-disodium hydrogen phosphate buffer, ammonia-ammonium chloride buffer, acetic acid-acetic acid
Sodium buffer, phosphate buffer solution, Tris-HCl buffer solution or HEPES buffer solution.
The concentration of the buffer solution is preferably 0.1mM~1M, can be 0.1mM, 0.5mM, 1mM, 5mM, 10mM,
100mM,1000mM；More preferably 10~100mM.
In step (2-1)：
Concentration of the mantoquita in the reaction system be 0.1mM~10mM, can be 0.1mM, 0.5mM,
0.75mM,1mM,5mM,10mM；Preferably 0.5~1mM；More preferably 0.75mM.
The pH is 3~10, can be 3,4,5,6,7,8,9,10；Preferably 6~8.
The temperature is 40~100 DEG C, can be 40 DEG C, 50 DEG C, 60 DEG C, 70 DEG C, 80 DEG C, 90 DEG C, 100 DEG C；It is preferred that
It is 60~100 DEG C.
The time is 1min~2h, can be 1min, 10min, 30min, 50min, 1h, 1.5h, 2h；Preferably
5min~1h.
In step (2-2)：
The strong acid is preferably one of hydrochloric acid, sulfuric acid, phosphoric acid and nitric acid or at least two.
The concentration of the strong acid is preferably 10M.
The dosage of the strong acid presses its concentration in hydrolysis reaction system preferably as 0.8~1.2M calculating；It is preferred that
For by its concentration in hydrolysis reaction system be 1M calculate.
The condition of the hydrolysis is preferably 90~100 DEG C of heating 30min~2h；Preferably 100 DEG C heating
60min。
The highly basic is preferably one or both of sodium hydroxide and potassium hydroxide.
The dosage of the highly basic preferably presses highly basic hydroxyl molal quantity：Hydrogen radical mole number of ions=1 of strong acid：1 meter
It calculates.
Concentration of the mantoquita in the reaction system be 0.1mM~10mM, can be 0.1mM, 0.5mM,
0.75mM,1mM,5mM,10mM；Preferably 0.5~1mM；More preferably 0.75mM.
The pH is 3~10, can be 3,4,5,6,7,8,9,10；Preferably 6~8.
The temperature is 40~100 DEG C, can be 40 DEG C, 50 DEG C, 60 DEG C, 70 DEG C, 80 DEG C, 90 DEG C, 100 DEG C；It is preferred that
It is 60~100 DEG C.
The time is 1min~2h, can be 1min, 10min, 30min, 50min, 1h, 1.5h, 2h；Preferably
5min~1h.
In step (2-2) (B)：
When the sample to be tested need to be added solvent and be dissolved and be diluted, solvent is water or buffer solution.
The buffer solution is preferably citric acid-disodium hydrogen phosphate buffer, ammonia-ammonium chloride buffer, acetic acid-acetic acid
Sodium buffer, phosphate buffer solution, Tris-HCl buffer solution or HEPES buffer solution.
The concentration of the buffer solution is preferably 0.1mM~1M, can be 0.1mM, 0.5mM, 1mM, 5mM, 10mM,
100mM,1000mM；More preferably 10~100mM.
A method of detection melamine and/or cyanuric acid, be according to above-mentioned mantoquita in detection melamine and/or
Application in cyanuric acid, the yet another aspect of proposition, includes the following steps：
When (3-1) carries out qualitative detection：
(3-1-1) when only whether detection sample to be tested contains cyanuric acid, steps are as follows：
(A) sample to be tested is configured to the solution of various concentration, copper salt solution is subsequently added into, obtains reaction system, one
A period of time is reacted under the conditions of fixed pH and temperature；
(B) when brown or brown color occurs in the solution of all various concentrations of preparation, tentatively judge testing sample solution
In do not contain cyanuric acid；When there are concentration solution present light blue or blue-green when, show in testing sample solution
Contain cyanuric acid；
(3-1-2) when only whether detection sample to be tested contains cyanuric acid and melamine, steps are as follows：
1. the processing of sample to be tested：
(A) a part of sample to be tested is taken, the testing sample solution of various concentration is configured to；
(B) a part of testing sample solution and strong acid are mixed, reaction is hydrolyzed；Then highly basic reaction is added, obtains
Treatment fluid；Treatment fluid is carried out to the diluted acid of certain gradient, is the treatment fluid of various concentration；
2. detecting：
(A) it is separately added into copper salt solution in the testing sample solution of various concentration, obtains reaction system, in certain pH
It is reacted for a period of time under the conditions of temperature, obtains a series of reaction solution A；
(B) it is separately added into copper salt solution in the treatment fluid of various concentration, obtains reaction system, in certain pH and temperature
Under the conditions of react a period of time, obtain a series of reaction solution B；
3. the judgement of result：
(A) when brown or brown color occur in all reaction solution A and all reaction solution B, tentatively judge sample to be tested
Cyanuric acid and melamine are not contained in solution；
(B) when brown or brown color occur in all reaction solution A, in a series of reaction solution B there are concentration
When light blue or blue-green is presented in reaction solution B, melamine is contained only in preliminary judgement sample solution；
(C) when there are the reaction solution A and the reaction solution B of concentration that has of concentration light blue or blue-green is presented when, feelings
Condition is specific as follows：
(a) when the light absorption value of reaction solution A and reaction solution B at 400nm of the test substance of homogenous quantities containing phase is identical, tentatively sentence
Disconnected sample to be tested is free of melamine containing only cyanuric acid；
(b) light absorption value as the reaction solution A and reaction solution B of the test substance of homogenous quantities containing phase at 400nm is reaction solution A >
Reaction solution B tentatively judges in sample to be tested containing melamine and cyanuric acid；
(3-2) includes the following steps when carrying out the quantitative detection：
(3-2-1) when only detecting the content of cyanuric acid in sample to be tested, steps are as follows：
(A) the cyanuric acid standard solution of various concentration is prepared, copper salt solution is added, reaction system is obtained, certain
A period of time is reacted under the conditions of pH and temperature, the measurement of light absorption value is carried out at 400nm, draws standard curve；
(B) copper salt solution is added in testing sample solution, obtains reaction system, it is anti-under the conditions of certain pH and temperature
It should a period of time；Then the measurement of light absorption value is carried out at 400nm, establishing criteria curve obtains cyanuric acid in sample to be tested
Content；
(3-2-2) when containing only melamine in sample to be tested, the step of melamine, is as follows in detection sample to be tested：
(A) melamine of various concentration and strong acid are mixed, reaction is hydrolyzed；Then highly basic reaction is added, obtains
Melamine treatment fluid；Copper salt solution is added in melamine treatment fluid, obtains reaction system, in certain pH and temperature strip
A period of time is reacted under part；Then the measurement that light absorption value is carried out at 400nm, draws standard curve；
(B) sample to be tested and strong acid are mixed, reaction is hydrolyzed；Then highly basic reaction is added, obtains at sample to be tested
Manage liquid；Copper salt solution is added in sample to be tested treatment fluid, obtains reaction system, reacts one under the conditions of certain pH and temperature
The section time；Then the measurement of light absorption value is carried out at 400nm, establishing criteria curve obtains containing for melamine in sample to be tested
Amount；
(3-2-3) detects melamine and three in sample to be tested when sample to be tested contains melamine and cyanuric acid
The step of paracyanogen acid is as follows：：
(A) according to step (3-2-1), the content of cyanuric acid is obtained；
(B) according to step (3-2-2), the total content of cyanuric acid and melamine is obtained；
(C) total content-cyanuric acid content of content=cyanuric acid of melamine and melamine.
In step (3-1-1) (A)：
The solvent of the preparation is water or buffer solution.
The buffer solution is preferably citric acid-disodium hydrogen phosphate buffer, ammonia-ammonium chloride buffer, acetic acid-acetic acid
Sodium buffer, phosphate buffer solution, Tris-HCl buffer solution or HEPES buffer solution.
The concentration of the buffer solution is preferably 0.1mM~1M, can be 0.1mM, 0.5mM, 1mM, 5mM, 10mM,
100mM,1000mM；More preferably 10~100mM.
Concentration of the mantoquita in the reaction system be 0.1mM~10mM, can be 0.1mM, 0.5mM,
0.75mM,1mM,5mM,10mM；Preferably 0.5~1mM；More preferably 0.75mM.
The pH is 3~10, can be 3,4,5,6,7,8,9,10；Preferably 6~8.
The temperature is 40~100 DEG C, can be 40 DEG C, 50 DEG C, 60 DEG C, 70 DEG C, 80 DEG C, 90 DEG C, 100 DEG C；It is preferred that
It is 60~100 DEG C.
The time is 1min~2h, can be 1min, 10min, 30min, 50min, 1h, 1.5h, 2h；Preferably
5min~1h.
Step (3-1-2) is 1. in (A)：
The solvent of the preparation is water or buffer solution.
The buffer solution is preferably citric acid-disodium hydrogen phosphate buffer, ammonia-ammonium chloride buffer, acetic acid-acetic acid
Sodium buffer, phosphate buffer solution, Tris-HCl buffer solution or HEPES buffer solution.
The concentration of the buffer solution is preferably 0.1mM~1M, can be 0.1mM, 0.5mM, 1mM, 5mM, 10mM,
100mM,1000mM；More preferably 10~100mM.
Step (3-1-2) is 1. in (B)：
The strong acid is preferably one of hydrochloric acid, sulfuric acid, phosphoric acid and nitric acid or at least two.
The concentration of the strong acid is preferably 10M.
The dosage of the strong acid presses its concentration in hydrolysis reaction system preferably as 0.8~1.2M calculating；It is preferred that
For by its concentration in hydrolysis reaction system be 1M calculate.
The condition of the hydrolysis is preferably 90~100 DEG C of heating 30min~2h；Preferably 100 DEG C heating
60min。
The highly basic is preferably one or both of sodium hydroxide and potassium hydroxide.
The dosage of the highly basic preferably presses highly basic hydroxyl molal quantity：Hydrogen radical mole number of ions=1 of strong acid：1 meter
It calculates.
Solvent used in the dilution is water or buffer solution.
The buffer solution is preferably citric acid-disodium hydrogen phosphate buffer, ammonia-ammonium chloride buffer, acetic acid-acetic acid
Sodium buffer, phosphate buffer solution, Tris-HCl buffer solution or HEPES buffer solution.
The concentration of the buffer solution is preferably 0.1mM~1M, can be 0.1mM, 0.5mM, 1mM, 5mM, 10mM,
100mM,1000mM；More preferably 10~100mM.
Step (3-1-2) 2. in：
Concentration of the mantoquita in the reaction system be 0.1mM~10mM, can be 0.1mM, 0.5mM,
0.75mM,1mM,5mM,10mM；Preferably 0.5~1mM；More preferably 0.75mM.
The pH is 3~10, can be 3,4,5,6,7,8,9,10；Preferably 6~8.
The temperature is 40~100 DEG C, can be 40 DEG C, 50 DEG C, 60 DEG C, 70 DEG C, 80 DEG C, 90 DEG C, 100 DEG C；It is preferred that
It is 60~100 DEG C.
The time is 1min~2h, can be 1min, 10min, 30min, 50min, 1h, 1.5h, 2h；Preferably
5min~1h.
In step (3-2-1) (A)：
The solvent of the preparation is water or buffer solution.
The buffer solution is preferably citric acid-disodium hydrogen phosphate buffer, ammonia-ammonium chloride buffer, acetic acid-acetic acid
Sodium buffer, phosphate buffer solution, Tris-HCl buffer solution or HEPES buffer solution.
The concentration of the buffer solution is preferably 0.1mM~1M, can be 0.1mM, 0.5mM, 1mM, 5mM, 10mM,
100mM,1000mM；More preferably 10~100mM.
In step (3-2-1) (B)：
When the sample to be tested need to be added solvent and be dissolved and be diluted, solvent is water or buffer solution.
The buffer solution is preferably citric acid-disodium hydrogen phosphate buffer, ammonia-ammonium chloride buffer, acetic acid-acetic acid
Sodium buffer, phosphate buffer solution, Tris-HCl buffer solution or HEPES buffer solution.
The concentration of the buffer solution is preferably 0.1mM~1M, can be 0.1mM, 0.5mM, 1mM, 5mM, 10mM,
100mM,1000mM；More preferably 10~100mM.
In step (3-2-1)：
Concentration of the mantoquita in the reaction system be 0.1mM~10mM, can be 0.1mM, 0.5mM,
0.75mM,1mM,5mM,10mM；Preferably 0.5~1mM；More preferably 0.75mM.
The pH is 3~10, can be 3,4,5,6,7,8,9,10；Preferably 6~8.
The temperature is 40~100 DEG C, can be 40 DEG C, 50 DEG C, 60 DEG C, 70 DEG C, 80 DEG C, 90 DEG C, 100 DEG C；It is preferred that
It is 60~100 DEG C.
The time is 1min~2h, can be 1min, 10min, 30min, 50min, 1h, 1.5h, 2h；Preferably
5min~1h.
In step (3-2-2)：
The strong acid is preferably one of hydrochloric acid, sulfuric acid, phosphoric acid and nitric acid or at least two.
The concentration of the strong acid is preferably 10M.
The dosage of the strong acid presses its concentration in hydrolysis reaction system preferably as 0.8~1.2M calculating；It is preferred that
For by its concentration in hydrolysis reaction system be 1M calculate.
The condition of the hydrolysis is preferably 90~100 DEG C of heating 30min~2h；Preferably 100 DEG C heating
60min。
The highly basic is preferably one or both of sodium hydroxide and potassium hydroxide.
The dosage of the highly basic preferably presses highly basic hydroxyl molal quantity：Hydrogen radical mole number of ions=1 of strong acid：1 meter
It calculates.
Concentration of the mantoquita in the reaction system be 0.1mM~10mM, can be 0.1mM, 0.5mM,
0.75mM,1mM,5mM,10mM；Preferably 0.5~1mM；More preferably 0.75mM.
The pH is 3~10, can be 3,4,5,6,7,8,9,10；Preferably 6~8.
The temperature is 40~100 DEG C, can be 40 DEG C, 50 DEG C, 60 DEG C, 70 DEG C, 80 DEG C, 90 DEG C, 100 DEG C；It is preferred that
It is 60~100
The time is 1min~2h, can be 1min, 10min, 30min, 50min, 1h, 1.5h, 2h；Preferably
5min~1h.
In step (3-2-2) (B)：
When the sample to be tested need to be added solvent and be dissolved and be diluted, solvent is water or buffer solution.
The buffer solution is preferably citric acid-disodium hydrogen phosphate buffer, ammonia-ammonium chloride buffer, acetic acid-acetic acid
Sodium buffer, phosphate buffer solution, Tris-HCl buffer solution or HEPES buffer solution.
The concentration of the buffer solution is preferably 0.1mM~1M, can be 0.1mM, 0.5mM, 1mM, 5mM, 10mM,
100mM,1000mM；More preferably 10~100mM.
Mantoquita above refers to soluble copper salt, preferably one in copper sulphate, copper acetate, copper chloride and copper nitrate
Kind or at least two.
The detection method can be used for detecting the content of melamine and/or cyanuric acid in actual sample.
The actual sample can be solid-state dairy products, liquid diary product, feed, blood, urine, tissue, swimming-pool water.
The principle of the present invention：When melamine or cyanuric acid are not present in solution to be measured, certain density mantoquita is molten
Liquid one time in certain pH and temperature can become brown from light blue, and this brown has in 400 rans
Very strong ultravioletvisible absorption.When, there are when melamine or cyanuric acid, certain density copper salt solution exists in solution to be measured
Certain buffer solution pH or without buffer solution and when temperature one time can keep light blue or slight variation occurs,
And it is this variation it is related with the content of melamine in solution or cyanuric acid, and it is this it is light blue in 400 rans without bright
Aobvious ultravioletvisible absorption.Based on the phenomenon, the situation of change of copper salt solution color can use, it is qualitative or semi-quantitatively survey
Determine melamine or cyanuric acid, the content of melamine or cyanuric acid quantitative determined using ultraviolet-uisible spectrophotometer,
The range of linearity of this method is 10nM~100M, preferably 10nM~1000nM.
The present invention has the following advantages and effects with respect to the prior art：
1. the present invention is based on inventors be surprised to learn that cyanuric acid molecule can inhibit the mantoquita to give birth under certain conditions
Copper oxide nanometer particle, the innovation and creation done are produced, and provide a kind of method for detecting melamine or cyanuric acid.
2. the method for the present invention is simple, cheaply, quickly, and sensitive (detection is limited to 10nM), specificity height, suitable for practical
The quick detection of melamine or cyanuric acid in sample.
3. having extensive present invention could apply to every field such as medicine, food or environmental test and determination techniques
Application prospect.
Detailed description of the invention
Fig. 1 is in embodiment 1 plus cyanuric acid and does not add the transmission electron microscope photo figure of cyanuric acid solution；Wherein, scheme A
For the solution for adding cyanuric acid；Scheming B is the solution for not adding cyanuric acid.
Fig. 2 is the solution thereon figure for adding cyanuric acid and do not add cyanuric acid of embodiment 1.
Fig. 3 is the spectral absorption curve figure of the solution of the melamine containing various concentration prepared by embodiment 5；Wherein, curve 1
For the solution without melamine, curve 2 is the solution of the melamine containing 1000nM.
Fig. 4 is canonical plotting prepared by embodiment 5.
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.
The measurement of 1 cyanuric acid of embodiment is computed, and the detectable concentration of the embodiment is 25nM, be converted into quality 25 ×
10-6×129.08×103=3.227mg/L is higher by residue criterion 2.5mg/KG
Accurate draw 0.1mL cyanuric acid solution (5mM) is added in ready 20mL colorimetric cylinder, then into colorimetric cylinder
It is added 1.5mL copper acetate solution (10mM), adds water constant volume to 20mL, obtain solution A.Accurate 0.1mL ultrapure water of drawing is added to
In ready 20mL colorimetric cylinder, then addition 1.5mL copper acetate solution (10mM) into colorimetric cylinder, add water constant volume to 20mL, obtains
To solution B.Solution A and solution B are heated 5 minutes at (80 DEG C) of water-bath, taken out.
With the substance in solution A and solution B of Japanese transmission electron microscope (JEM-2100F) detection after heat-treated
Pattern.As shown in Figure 1, the results showed that in the presence of cyanuric acid, no nano particle forms (ie in solution A)；When no cyanuric acid
When, there is nano particle to form (ie in solution B).
As shown in Fig. 2, solution is in light blue (ie in solution A) in the presence of cyanuric acid；When no cyanuric acid, solution
In brown color.Therefore cyanuric acid (ie in solution B) can be detected by color change.
The measurement of 2 melamine of embodiment
(1) sample treatment：
Melamine sample treatment：Accurate draw 1.25mL melamine solution (40mM) is added in 10mL colorimetric cylinder, adds
Enter the sulfuric acid solution boiling water bath 1h that 1mL concentration is 10M, place room temperature, the sodium hydroxide solution that 1mL concentration is 20M is added, adds water
It is settled to 10mL, obtains melamine treatment fluid.
Blank sample processing：Accurate 1.25mL water of drawing is added in 10mL colorimetric cylinder, and the sulfuric acid that 1mL concentration is 10M is added
Solution boiling water bath 1h places room temperature, and the sodium hydroxide solution that 1mL concentration is 20M is added, adds water to be settled to 10mL, obtains blank
Sample treatment liquid.
(2) it detects：Accurate 0.1mL melamine treatment fluid of drawing is added in ready 20mL colorimetric cylinder, then toward than
1.5mL copper acetate solution (10mM) is added in colour tube, (100mM NaAc, is adjusted with acetic acid with the acetate buffer solution of pH7.0
PH be 7) constant volume to 20mL.Accurate 0.1mL blank sample treatment fluid of drawing is added in ready 20mL colorimetric cylinder, then toward than
1.5mL copper acetate solution (10mM) is added in colour tube, (100mM NaAc, is adjusted with acetic acid with the acetate buffer solution of pH7.0
PH be 7) constant volume to 20mL.(70 DEG C) of water-bath are heated 10 minutes, are taken out.
(3) the result shows that, melamine processing liquor is added and keeps blue, blank sample processing liquor, which is added, to be become
Brown color.Therefore, melamine can be detected by color change.
Embodiment 3 selectively measures
(1) sample treatment：It is accurate to draw 1.25mL melamine solution (40mM), 1.25mL cyanuric acid solution
(40mM), 1.25mL uric acid solution (40mM), 1.25mL urea liquid (40mM), 1.25mL dicyandiamide solution (40mM),
1.25mL ammonia spirit (40mM), is separately added into 10mL colorimetric cylinder, and the sulfuric acid solution boiling water bath 1h that 1mL concentration is 10M is added,
Room temperature is placed, the sodium hydroxide solution that 1mL concentration is 20M is added, water is added to be settled to 10mL.
(2) it detects：Each sample processing solution is added separately to ready 20mL ratio in accurate absorption 0.1mL the present embodiment
In colour tube, then it is separately added into 1.5mL copper acetate solution (10mM) into colorimetric cylinder, adds the acetate buffer solution (10mM of pH8.0
NaAc is 8) constant volume to 20mL with vinegar acid for adjusting pH.(60 DEG C) of water-bath are heated 1 hour, are taken out.
(3) the result shows that, the processing liquor that melamine and cyanuric acid is added keeps blue, and other samples are added
Processing liquor becomes brown color.Therefore, it can determine that this method has selectivity well by color change.
The measurement of 4 interference of embodiment
It is accurate respectively to draw 0.1mL cyanuric acid solution (5mM), it is added in ready 7 20mL colorimetric cylinders, then past
1.5mL copper acetate solution (10mM) is added in each colorimetric cylinder, 1mL water, 1mLNaCl is added into 7 colorimetric cylinders again respectively
(1mM)、1mLMgSO4(1mM)、1mL FeSO4(1mM)、1mL FeCl3(1mM)、1mL NH4NO3(1mM), 1mL zinc acetate
(1mM) adds water constant volume to 20mL.(100 DEG C) of water-bath are heated 1 minute, are taken out.
As a result such as table 1, it is seen that this method has good anti-interference.
Table 1
| Water | NaCl | MgSO4 | FeSO4 | FeCl3 | NH4NO3 | Zinc acetate |
| It is light blue | It is light blue | It is light blue | It is light blue | It is light blue | It is light blue | It is light blue |
The measurement of melamine in 5 milk powder of embodiment
(1) sample treatment：
Melamine sample treatment：It is accurate draw 1.25mL melamine solution (0 μM, 16 μM, 160 μM, 1.6mM,
16mM, 160mM) it is added in the colorimetric cylinder of 10mL, the sulfuric acid solution boiling water bath 1h that 1mL concentration is 10M is added, places room temperature, adds
Enter the sodium hydroxide solution that 1mL concentration is 20M, water is added to be settled to 10mL.
Powdered milk sample processing：It accurately weighs 1.25g milk powder (Erie's board milk powder) to be added in 10mL colorimetric cylinder, it is dense that 1mL is added
Degree is the sulfuric acid solution boiling water bath 1h of 10M, places room temperature, and the sodium hydroxide solution that 1mL concentration is 20M is added, water is added to be settled to
10mL, filtering.
Respectively it is accurate draw various concentration in 0.1mL the present embodiment melamine processing solution (0 μM, 2 μM, 20 μM,
200 μM, 2mM, 20mM) it is added in ready 7 20mL colorimetric cylinders, then the copper acetate of addition 1.5mL is molten into colorimetric cylinder
Liquid (10mM), add pH8.0 Tris-HCl buffer solution (10mM Tris, with HCl adjust pH be 8) constant volume to 20mL.Water-bath
(80 DEG C) are heated 10 minutes, are taken out.It is bent using absorption of the ultraviolet-uisible spectrophotometer measurement solution at 250nm~750nm
Line, as shown in figure 3, the concentration of curve therein 1,2 corresponding melamines is 0nM, 1000nM.It chooses at 400nm
Absorbance is measuring point, and measuring melamine concentration respectively is 10nM, 50nM, 100nM, 500nM, 1000nM at 400nm
Absorbance draws standard curve, as shown in Figure 4.
(2) it detects：
Accurate 0.1mL milk powder treatment fluid of drawing is added in ready 20mL colorimetric cylinder, then is added into colorimetric cylinder
The copper acetate solution (10mM) of 1.5mL, with the Tris-HCl buffer solution constant volume of pH8.0 to 20mL.(80 DEG C) of water-bath heating 10
Minute, it takes out.Using absorbance of the ultraviolet-uisible spectrophotometer measurement solution at 400nm, absorbance value is substituted into and is returned
Equation can calculate the content of melamine in milk powder.The result shows that the content of melamine is 0 in the milk powder.
The measurement of cyanuric acid in 6 swimming-pool water of embodiment
(1) sample treatment：
The accurate cyanuric acid solution (0 μM, 2 μM, 20 μM, 200 μM, 2mM, 20mM) for drawing 0.1mL various concentration respectively
It is added in ready 7 20mL colorimetric cylinders, then 1.5mL copper acetate solution (10mM) is added into colorimetric cylinder, add pH8.0's
Phosphate buffer solution (10mM NaH2PO4, with phosphoric acid solution by pH be adjusted to 8.0) constant volume to 20mL.(80 DEG C) of water-bath heating
It 10 minutes, takes out.Using absorbance of the ultraviolet-uisible spectrophotometer measurement solution at 400nm, standard curve is drawn.
The accurate 0.1mL that draws is added in ready 20mL colorimetric cylinder through the swimming-pool water of filtration treatment, then toward colorimetric
1.5mL copper acetate solution (10mM) is added in pipe, with phosphate buffer solution (the 10mM NaH of pH8.02PO4, use phosphoric acid solution
By pH be adjusted to 8.0) constant volume to 20mL.(80 DEG C) of water-bath are heated 10 minutes, are taken out.It is measured using ultraviolet-uisible spectrophotometer
Absorbance of the solution at 400nm, substitutes into regression equation for absorbance value, can calculate the content of cyanuric acid in swimming pool.Knot
Fruit shows that the content of cyanuric acid in the swimming pool is 0.
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. application of the mantoquita in detection melamine and/or cyanuric acid.
2. application of the mantoquita according to claim 1 in detection melamine and/or cyanuric acid, it is characterised in that：
The mantoquita is one of copper sulphate, copper acetate, copper chloride and copper nitrate or at least two.
3. application of the mantoquita according to claim 1 or 2 in detection melamine and/or cyanuric acid, feature exist
In：Described is detected as one or both of qualitative detection and quantitative detection.
4. application of the mantoquita according to claim 3 in detection melamine and/or cyanuric acid, it is characterised in that：
When carrying out the qualitative detection, include the following steps：
(1-1) when only whether detection sample to be tested contains cyanuric acid, steps are as follows：
(A) sample to be tested is configured to the solution of various concentration, copper salt solution is subsequently added into, obtains reaction system, certain
A period of time is reacted under the conditions of pH and temperature；
(B) when brown or brown color occurs in the solution of all various concentrations of preparation, tentatively judge in testing sample solution not
Contain cyanuric acid；When there are concentration solution keep present light blue or blue-green when, show in testing sample solution
Contain cyanuric acid；
(1-2) when only whether detection sample to be tested contains cyanuric acid and melamine, steps are as follows：
1. the processing of sample to be tested：
(A) a part of sample to be tested is taken, the testing sample solution of various concentration is configured to；
(B) a part of testing sample solution and strong acid are mixed, reaction is hydrolyzed；Then highly basic reaction is added, is handled
Liquid；Treatment fluid is carried out to the dilution of certain gradient, is the treatment fluid of various concentration；
2. detecting：
(A) it is separately added into copper salt solution in the testing sample solution of various concentration, obtains reaction system, in certain pH and temperature
A period of time is reacted under the conditions of degree, obtains a series of reaction solution A；
(B) it is separately added into copper salt solution in the treatment fluid of various concentration, obtains reaction system, in certain pH and temperature condition
Lower reaction a period of time, obtain a series of reaction solution B；
3. the judgement of result：
(A) when brown or brown color occur in all reaction solution A and all reaction solution B, tentatively judge testing sample solution
In do not contain cyanuric acid and melamine；
(B) when brown or brown color occur in all reaction solution A, in a series of reaction solution B there are concentration reaction
When blue-green or blue-green is presented in liquid B, melamine is contained only in preliminary judgement sample solution；
(C) when there are the reaction solution A and the reaction solution B of concentration that has of concentration blue-green or blue-green is presented when, situation tool
Body is as follows：
(a) when the light absorption value of reaction solution A and reaction solution B at 400nm of the test substance of homogenous quantities containing phase is identical, tentatively judge to
Sample is free of melamine containing only cyanuric acid；
(b) light absorption value as the reaction solution A and reaction solution B of the test substance of homogenous quantities containing phase at 400nm is reaction solution A > reaction
Liquid B tentatively judges in sample to be tested containing melamine and cyanuric acid；
When carrying out the quantitative detection, include the following steps：
(2-1) when only detecting the content of cyanuric acid in sample to be tested, steps are as follows：
(A) the cyanuric acid standard solution for preparing various concentration, is added copper salt solution, obtains reaction system, in certain pH and
A period of time is reacted under the conditions of temperature, the measurement of light absorption value is carried out at 400nm, draws standard curve；
(B) copper salt solution is added in testing sample solution, obtains reaction system, reacts one under the conditions of certain pH and temperature
The section time；Then the measurement of light absorption value is carried out at 400nm, establishing criteria curve obtains containing for cyanuric acid in sample to be tested
Amount；
(2-2) when containing only melamine in sample to be tested, the step of melamine, is as follows in detection sample to be tested：
(A) melamine of various concentration and strong acid are mixed, reaction is hydrolyzed；Then highly basic reaction is added, obtains trimerization
Cyanamide treatment fluid；Copper salt solution is added in melamine treatment fluid, obtains reaction system, under the conditions of certain pH and temperature
Reaction a period of time；Then the measurement that light absorption value is carried out at 400nm, draws standard curve；
(B) testing sample solution and strong acid are mixed, reaction is hydrolyzed；Then highly basic reaction is added, obtains at sample to be tested
Manage liquid；Copper salt solution is added in sample to be tested treatment fluid, obtains reaction system, reacts one under the conditions of certain pH and temperature
The section time；Then the measurement of light absorption value is carried out at 400nm, establishing criteria curve obtains containing for melamine in sample to be tested
Amount；
(2-3) detects melamine and cyanuric acid in sample to be tested when sample to be tested contains melamine and cyanuric acid
The step of it is as follows：
(A) according to step (2-1), the content of cyanuric acid is obtained；
(B) according to step (2-2), the total content of cyanuric acid and melamine is obtained；
(C) total content-cyanuric acid content of content=cyanuric acid of melamine and melamine.
5. application of the mantoquita according to claim 4 in detection melamine and/or cyanuric acid, it is characterised in that：
Step (1-1) (A), step (1-2) 1. (A), in step (2-1) (A)：
The solvent of the preparation is water or buffer solution；
Step (1-1) (A), step (1-2) 2., in step (2-1)：
Concentration of the mantoquita in the reaction system is 0.1mM~10mM；
The pH is 3~10；
The temperature is 40~100 DEG C；
The time is 1min~2h；
Step (1-2) 1. (B), in step (2-2)：
The strong acid is one of hydrochloric acid, sulfuric acid, phosphoric acid and nitric acid or at least two；
The dosage of the strong acid is 0.8~1.2M calculating by its concentration in hydrolysis reaction system；
The condition of the hydrolysis is 90~100 DEG C of heating 30min~2h；
The highly basic is one or both of sodium hydroxide and potassium hydroxide；
The dosage of the highly basic presses highly basic hydroxyl molal quantity：Hydrogen radical mole number of ions=1 of strong acid：1 calculates；
Step (1-2) is 1. in (B)：
Solvent used in the dilution is water or buffer solution；
In step (2-1) (B) and step (2-2) (B)：
When the sample to be tested need to be added solvent and be dissolved and be diluted, solvent is water or buffer solution.
6. application of the mantoquita according to claim 5 in detection melamine and/or cyanuric acid, it is characterised in that：
The buffer solution is citric acid-disodium hydrogen phosphate buffer, ammonia-ammonium chloride buffer, Acetic acid-sodium acetate buffering
Liquid, phosphate buffer solution, Tris-HCl buffer solution or HEPES buffer solution；
Concentration of the mantoquita in the reaction system is 0.5~1mM；
The pH is 6~8；
The temperature is 60~100 DEG C；
The time is 5min~1h；
The dosage of the strong acid is 1M calculating by its concentration in hydrolysis reaction system；
The condition of the hydrolysis is 100 DEG C of heating 60min.
7. a kind of method of detection melamine and/or cyanuric acid, it is characterised in that include the following steps：
When (3-1) carries out qualitative detection：
(3-1-1) when only whether detection sample to be tested contains cyanuric acid, steps are as follows：
(A) sample to be tested is configured to the solution of various concentration, copper salt solution is subsequently added into, obtains reaction system, certain
A period of time is reacted under the conditions of pH and temperature；
(B) when brown or brown color occurs in the solution of all various concentrations of preparation, tentatively judge in testing sample solution not
Contain cyanuric acid；When there are concentration solution present light blue or blue-green when, show to contain in testing sample solution
Cyanuric acid；
(3-1-2) when only whether detection sample to be tested contains cyanuric acid and melamine, steps are as follows：
1. the processing of sample to be tested：
(A) a part of sample to be tested is taken, the testing sample solution of various concentration is configured to；
(B) a part of testing sample solution and strong acid are mixed, reaction is hydrolyzed；Then highly basic reaction is added, is handled
Liquid；Treatment fluid is carried out to the diluted acid of certain gradient, is the treatment fluid of various concentration；
2. detecting：
(A) it is separately added into copper salt solution in the testing sample solution of various concentration, obtains reaction system, in certain pH and temperature
A period of time is reacted under the conditions of degree, obtains a series of reaction solution A；
(B) it is separately added into copper salt solution in the treatment fluid of various concentration, obtains reaction system, in certain pH and temperature condition
Lower reaction a period of time, obtain a series of reaction solution B；
3. the judgement of result：
(A) when brown or brown color occur in all reaction solution A and all reaction solution B, tentatively judge testing sample solution
In do not contain cyanuric acid and melamine；
(B) when brown or brown color occur in all reaction solution A, in a series of reaction solution B there are concentration reaction
When light blue or blue-green is presented in liquid B, melamine is contained only in preliminary judgement sample solution；
(C) when there are the reaction solution A and the reaction solution B of concentration that has of concentration light blue or blue-green is presented when, situation tool
Body is as follows：
(a) when the light absorption value of reaction solution A and reaction solution B at 400nm of the test substance of homogenous quantities containing phase is identical, tentatively judge to
Sample is free of melamine containing only cyanuric acid；
(b) light absorption value as the reaction solution A and reaction solution B of the test substance of homogenous quantities containing phase at 400nm is reaction solution A > reaction
Liquid B tentatively judges in sample to be tested containing melamine and cyanuric acid；
(3-2) includes the following steps when carrying out the quantitative detection：
(3-2-1) when only detecting the content of cyanuric acid in sample to be tested, steps are as follows：
(A) prepare the cyanuric acid standard solution of various concentration, copper salt solution be added, obtains reaction system, in certain pH and
A period of time is reacted under the conditions of temperature, the measurement of light absorption value is carried out at 400nm, draws standard curve；
(B) copper salt solution is added in testing sample solution, obtains reaction system, reacts one under the conditions of certain pH and temperature
The section time；Then the measurement of light absorption value is carried out at 400nm, establishing criteria curve obtains containing for cyanuric acid in sample to be tested
Amount；
(3-2-2) when containing only melamine in sample to be tested, the step of melamine, is as follows in detection sample to be tested：
(A) melamine of various concentration and strong acid are mixed, reaction is hydrolyzed；Then highly basic reaction is added, obtains trimerization
Cyanamide treatment fluid；Copper salt solution is added in melamine treatment fluid, obtains reaction system, under the conditions of certain pH and temperature
Reaction a period of time；Then the measurement that light absorption value is carried out at 400nm, draws standard curve；
(B) sample to be tested and strong acid are mixed, reaction is hydrolyzed；Then highly basic reaction is added, obtains sample to be tested treatment fluid；
Copper salt solution is added in sample to be tested treatment fluid, obtains reaction system, when reacting one section under the conditions of certain pH and temperature
Between；Then the measurement of light absorption value is carried out at 400nm, establishing criteria curve obtains the content of melamine in sample to be tested；
(3-2-3) detects melamine and melamine in sample to be tested when sample to be tested contains melamine and cyanuric acid
The step of acid is as follows：：
(A) according to step (3-2-1), the content of cyanuric acid is obtained；
(B) according to step (3-2-2), the total content of cyanuric acid and melamine is obtained；
(C) total content-cyanuric acid content of content=cyanuric acid of melamine and melamine.
8. the method in detection melamine according to claim 7 and/or cyanuric acid, it is characterised in that：
Step (3-1-1) (A), step (3-1-2) 1. (A), in step (3-2-1) (A)：
The solvent of the preparation is water or buffer solution；
Step (3-1-1) (A), step (3-1-2) 2., in step (3-2-1)：
Concentration of the mantoquita in the reaction system is 0.1mM~10mM；
The pH is 3~10；
The temperature is 40~100 DEG C；
The time is 1min~2h；
Step (3-1-2) 1. (B), in step (3-2-2)：
The strong acid is one of hydrochloric acid, sulfuric acid, phosphoric acid and nitric acid or at least two；
The dosage of the strong acid is 0.8~1.2M calculating by its concentration in hydrolysis reaction system；
The condition of the hydrolysis is 90~100 DEG C of heating 30min~2h；
The highly basic is one or both of sodium hydroxide and potassium hydroxide；
The dosage of the highly basic presses highly basic hydroxyl molal quantity：Hydrogen radical mole number of ions=1 of strong acid：1 calculates；
Step (3-1-2) is 1. in (B)：
Solvent used in the dilution is water or buffer solution；
In step (3-2-1) (B) and step (3-2-2) (B)：
When the sample to be tested need to be added solvent and be dissolved and be diluted, solvent is water or buffer solution.
9. detection method described in claim 7 or 8 is detected in actual sample in the content of melamine and/or cyanuric acid
Application.
10. application according to claim 9, it is characterised in that：The actual sample is solid-state dairy products, liquid milk system
Product, feed, blood, urine, tissue or swimming-pool water.
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| CN103558336A (en) * | 2013-10-24 | 2014-02-05 | 中国科学院宁波材料技术与工程研究所 | Portable food safety inspection reagent as well as preparation method and application thereof |
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