CN109856348A - A kind of method of melamine in quick measurement meat - Google Patents
A kind of method of melamine in quick measurement meat Download PDFInfo
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- CN109856348A CN109856348A CN201910174962.1A CN201910174962A CN109856348A CN 109856348 A CN109856348 A CN 109856348A CN 201910174962 A CN201910174962 A CN 201910174962A CN 109856348 A CN109856348 A CN 109856348A
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Abstract
The invention discloses a kind of methods of melamine in quickly measurement meat, particularly belong to detection field, this method comprises the following steps: by meat sample homogenization to be measured, and protein precipitant and grease removal agent is added, and after the completion of purification reaction, chilled centrifugal treating, filtering, obtains refined solution.Adsorbent is added in refined solution, is ultrasonically treated 20 ~ 30min, obtains solidliquid mixture.Solid absorbent is separated using magnetisable material, obtains adsorbent and extraction raffinate.It is attached with the adsorbent of adsorbate using Acidifying acetonitrile elution, obtains eluent.Eluent is rotated to doing, and residue is obtained.Residue is redissolved with pregnant solution, and filtering obtains filter liquor.In obtained filter liquor, formaldehyde, inorganic base are sequentially added, reacts 60 ~ 90min under conditions of 75 DEG C after shaking up dissolution, after test drug is added, drug developing is tested, then shows to contain melamine in meat sample.Method provided by the invention has the advantages that easy to operate and can quickly detect.
Description
Technical field
The invention belongs to detection field, the method for melamine in specially a kind of quickly measurement meat.
Background technique
In in September, 2008, most country's famous brand name milk powder discoveries are polluted by melamine.Country takes at once accordingly to be arranged
It applies, raw milk and melamine in dairy products detection national standard has been put into effect at the beginning of 10 months 2008.For in food and feed
Melamine detection research focuses primarily upon in recent years, and some criminals utilize the loophole of existing protein content analysis, in order to mention
High feed and food detection in protein content and maliciously add melamine thereto, bad influence is caused to society.
It is mainly in the prior art high performance liquid chromatography, liquid chromatography mass for measuring the analysis method of melamine
Method and liquid chromatogram-tandem mass spectrometry, wherein with the most commonly used of high performance liquid chromatography.However, above-mentioned for measuring
The analysis method of melamine has the following disadvantages: the requirement that the process of above-mentioned analysis detection is complex, to laboratory condition
It is higher.Also, traditional detection method is mostly quantitative detection, and not only time-consuming for quantitative detection, is unfavorable for for high-volume sample
Product are detected.
Summary of the invention
The present invention provides a kind of method of melamine in quickly measurement meat, this method has easy to operate and can
Quickly the advantages of detection.
To achieve the above object, the invention provides the following technical scheme:
A kind of method of melamine in quick measurement meat, this method comprises the following steps:
(1) qualitative detection of melamine
(1.1) by meat sample homogenization to be measured, slurries are obtained；
(1.2) it is added protein precipitant and grease removal agent in obtained slurries, after the completion of purification reaction, chilled centrifugal treating,
Filtering, obtains refined solution；
(1.3) adsorbent made of magnetic composite is added in refined solution, is ultrasonically treated 20 ~ 30min, it is mixed to obtain solid-liquid
Close object；
(1.4) solid absorbent in solidliquid mixture is separated using magnetisable material, obtains the suction for being adsorbed with adsorbate
Attached dose and extraction raffinate；
(1.5) it is attached with the adsorbent of adsorbate using Acidifying acetonitrile elution, obtains eluent and solid absorbent；Extraction raffinate is abandoned
It goes；
(1.6) eluent is rotated to doing, and obtains residue；Solid absorbent is through pure water clean and reuse；
(1.7) residue is taken, is redissolved with pregnant solution, filters, obtains filter liquor；
(1.8) in obtained filter liquor, formaldehyde, inorganic base are sequentially added, is reacted under conditions of 60 ~ 80 DEG C after shaking up dissolution
60 ~ 90min obtains test solution；
(1.9) test drug is added in test solution, tests drug developing, then shows to contain melamine in meat sample；
Otherwise, show in meat sample without containing melamine.
Preferably, pregnant solution is selected from any one of ethylene glycol or pyridine in step (1.7).
Preferably, inorganic base is any in potassium hydroxide, Kocide SD and sodium carbonate in step (1.8)
It is a kind of.
Preferably, reaction temperature is 75 DEG C, reaction time 80min in step (1.8).
Preferably, inorganic base is selected from any one of potassium hydroxide or sodium carbonate, then in step (1.9): test medicine
Product select metallic sodium or metallic potassium.
Preferably, inorganic base is selected from Kocide SD, then in step (1.9): test drug selects potassium iodide.
Preferably, in step (1.2), any one of protein precipitant in acetonitrile, acetone；Grease removal agent is selected from
N-hexane and C18In any one.
Preferably, adsorbent is selected from chitosan and nanometer Fe in step (1.3)3O4Cross-linking products, CoFe2O4-
Any one in graphene nanocomposite material.
Preferably, any one or it of the crosslinking agent in glutaraldehyde, formaldehyde, epoxychloropropane, beta-cyclodextrin
Mixture.
Preferably, further include step (2) after step (1.9), the step (2) are as follows:
(2) quantitative detection of melamine
(2.1) in obtained residue, be added buffer solution redissolve, be added antibacterial agent, and successively be added derivatization reagent with it is interior
Solution is marked, oscillation to reaction is completed, and filtering and is settled to 1ml, the object to be detected for the analysis that obtains being available on the machine；
Wherein, antibacterial agent is selected from least one of titanium dioxide, zinc oxide or chitosan.
Preferably, chitosan and nanometer Fe3O4The preparation methods of cross-linking products include the following steps:
S01, chitosan is immersed in crosslinking agent, and be stirred continuously, continue 60 ~ 120min, filtered, obtain being adsorbed with crosslinking agent
Chitosan；
S02, nanometer Fe is added in the chitosan for being adsorbed with crosslinking agent3O4, under the conditions of 60 ~ 80 DEG C of temperature, it is stirred continuously
30 ~ 50min to get arrive chitosan and nanometer Fe3O4Cross-linking products.
Preferably, buffer solution is 0.1mol/L triethylamine-carbonate buffer solution in step (2.1).
Preferably, derivatization reagent is the 2- nitrobenzaldehyde dimethyl sulfoxide solution of 10mg/L.
The invention has the benefit that
In the present invention, extracted dose of meat sample of extraction, the melamine contained inside it, lipid and albumen is precipitated
The components such as matter.And extracting solution is handled through grease removal and removing protein, obtains refined solution after purification.Refined solution is melamine and extraction
The mixture of agent, wherein a small amount of impurity contained is negligible.Refined solution, can be by melamine rich by the absorption of adsorbent.
Therefore, there is melamine in obtained residue, also there are other impurity, in order to further purify impurity, richness is can be used in residue
Collect agent to redissolve, so that melamine exists in the form of higher concentration.After obtaining more pure melamine solution, pass through
Reaction, and using the detection of test drug, make its developing.Then, technical staff can according to developing it is qualitative obtain in sample whether
Contain melamine.Qualitative detection is carried out to the solution in sample by the above method, experimenter can be accelerated to meat sample
The screening of quality, so that detection efficiency is higher.
Specific embodiment
Embodiment 1
A kind of method of melamine in quick measurement meat, this method comprises the following steps:
(1) qualitative detection of melamine
(1.1) by meat sample homogenization to be measured, slurries are obtained.
(1.2) it is added acetonitrile and n-hexane in obtained slurries, after the completion of purification reaction, chilled centrifugal treating, mistake
Filter, obtains refined solution.Can further extracting solution be purified by removing protein and fat.
(1.3) CoFe is added in refined solution2O4Graphene nanocomposite material is ultrasonically treated 25min, and it is mixed to obtain solid-liquid
Close object.
(1.4) using magnetisable material to CoFe2O4Graphene nanocomposite material is separated, and obtains being adsorbed with adsorbate
CoFe2O4Graphene nanocomposite material and extraction raffinate.
(1.5) CoFe of adsorbate is attached with using Acidifying acetonitrile elution2O4Graphene nanocomposite material is eluted
Liquid and CoFe2O4Graphene nanocomposite material.Extraction raffinate discards.
(1.6) eluent is rotated to doing, and obtains residue；CoFe2O4Graphene nanocomposite material is through pure water
Clean and reuse.
(1.7) residue is taken, spent glycol redissolves, and filtering obtains filter liquor.It selects and is the reason of ethylene glycol herein, three
Solubility of the poly cyanamid in ethylene glycol is very high, can play the role of enrichment.
(1.8) in obtained filter liquor, formaldehyde, potassium hydroxide are sequentially added, is shaken up after dissolving under conditions of 75 DEG C
80min is reacted, test solution is obtained.Since potassium hydroxide is also that can dissolve, therefore can be entire reactant in ethylene glycol
Alkalinity is presented in system, reaction principle such as following formula:
(1.9) metallic sodium is added in test solution, tests drug developing, shows to contain in meat sample if generating bubble
Melamine；Otherwise, bubble is not generated to show in meat sample without containing melamine.
Embodiment 2
The present embodiment is further elaborated on the basis of embodiment 1:
The result obtained in the embodiment 1 are as follows: contain melamine in meat sample.It then needs to carry out following steps:
In the residue obtained in 1 step of embodiment (1.6), 0.1mol/L triethylamine-carbonate buffer solution is added and redissolves, is added
Chitosan, and derivatization reagent and inner mark solution is successively added, oscillation to reaction is completed, filtering, and is settled to 1ml, and obtaining can
The object to be detected of upper machine analysis.The effect of chitosan is, can play antibacterial effect, prevents the impurity in sample solution from breeding
Microorganism, to influence testing result.And chitosan is relatively insoluble in general solvent, can be removed by filtration, and will not influence inspection
Survey result.
Although the present invention is described in detail referring to the foregoing embodiments, for those skilled in the art,
It is still possible to modify the technical solutions described in the foregoing embodiments, or part of technical characteristic is carried out etc.
With replacement, all within the spirits and principles of the present invention, any modification, equivalent replacement, improvement and so on should be included in this
Within the protection scope of invention.
Claims (10)
1. a kind of method of melamine in quickly measurement meat, which comprises the steps of:
(1) qualitative detection of melamine
(1.1) by meat sample homogenization to be measured, slurries are obtained；
(1.2) it is added protein precipitant and grease removal agent in obtained slurries, after the completion of purification reaction, chilled centrifugal treating,
Filtering, obtains refined solution；
(1.3) adsorbent made of magnetic composite is added in refined solution, is ultrasonically treated 20 ~ 30min, it is mixed to obtain solid-liquid
Close object；
(1.4) solid absorbent in solidliquid mixture is separated using magnetisable material, obtains the suction for being adsorbed with adsorbate
Attached dose and extraction raffinate；
(1.5) it is attached with the adsorbent of adsorbate using Acidifying acetonitrile elution, obtains eluent and solid absorbent；Extraction raffinate is abandoned
It goes；
(1.6) eluent is rotated to doing, and obtains residue；Solid absorbent is through pure water clean and reuse；
(1.7) residue is taken, is redissolved with pregnant solution, filters, obtains filter liquor；
(1.8) in obtained filter liquor, formaldehyde, inorganic base are sequentially added, is reacted under conditions of 60 ~ 80 DEG C after shaking up dissolution
60 ~ 90min obtains test solution；
(1.9) test drug is added in test solution, tests drug developing, then shows to contain melamine in meat sample；
Otherwise, show in meat sample without containing melamine.
2. the method for melamine in a kind of quickly measurement meat according to claim 1, which is characterized in that in step
(1.7) in, pregnant solution is selected from any one of ethylene glycol or pyridine.
3. the method for melamine in a kind of quickly measurement meat according to claim 1, which is characterized in that in step
(1.8) in, any one of inorganic base in potassium hydroxide, Kocide SD and sodium carbonate.
4. the method for melamine in a kind of quickly measurement meat according to claim 1, which is characterized in that in step
(1.8) in, reaction temperature is 75 DEG C, reaction time 80min.
5. the method for melamine in a kind of quickly measurement meat according to claim 3, which is characterized in that in step
(1.9) in, inorganic base is selected from any one of potassium hydroxide or sodium carbonate, then: test drug selects metallic sodium or metallic potassium.
6. the method for melamine in a kind of quickly measurement meat according to claim 3, which is characterized in that in step
(1.9) in, inorganic base is selected from Kocide SD, then: test drug selects potassium iodide.
7. the method for melamine in a kind of quickly measurement meat according to claim 1, which is characterized in that in step
(1.2) in, any one of protein precipitant in acetonitrile, acetone；
Grease removal agent is selected from n-hexane and C18In any one.
8. the method for melamine in a kind of quickly measurement meat according to claim 1, which is characterized in that in step
(1.3) in, adsorbent is selected from chitosan and nanometer Fe3O4Cross-linking products, CoFe2O4Appointing in graphene nanocomposite material
It anticipates one kind.
9. the method for melamine in a kind of quickly measurement meat according to claim 1, which is characterized in that crosslinking agent choosing
Mixture from any one or they in glutaraldehyde, formaldehyde, epoxychloropropane, beta-cyclodextrin.
10. the method for melamine in a kind of quickly measurement meat according to claim 1, which is characterized in that in step
It (1.9) further include step (2) after, the step (2) are as follows:
(2) quantitative detection of melamine
(2.1) in obtained residue, be added buffer solution redissolve, be added antibacterial agent, and successively be added derivatization reagent with it is interior
Solution is marked, oscillation to reaction is completed, and filtering and is settled to 1ml, the object to be detected for the analysis that obtains being available on the machine；
Wherein, antibacterial agent is selected from least one of titanium dioxide, zinc oxide or chitosan.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111521458A (en) * | 2020-04-21 | 2020-08-11 | 深圳市深大检测有限公司 | Method for detecting liquid milk melamine |
Citations (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101387609A (en) * | 2008-10-20 | 2009-03-18 | 中国农业大学 | Method for rapidly detecting melamine |
| CN101576544A (en) * | 2009-04-21 | 2009-11-11 | 新疆出入境检验检疫局检验检疫技术中心 | Method for fast detecting melamine in cream biscuit |
| CN101576543A (en) * | 2009-04-21 | 2009-11-11 | 新疆出入境检验检疫局检验检疫技术中心 | Method for fast detecting melamine in dry milk |
| WO2010090751A2 (en) * | 2009-02-05 | 2010-08-12 | The Regents Of The University Of California | Methods and materials for the detection of melamine |
| CN101968452A (en) * | 2010-03-05 | 2011-02-09 | 浙江省疾病预防控制中心 | Kit for quickly detecting tripolycyanamide and use thereof |
| CN102827321A (en) * | 2012-09-06 | 2012-12-19 | 同济大学 | Preparation method and application for magnetic molecularly imprinted polymers for selectively separating carbamazepine |
| CN102879504A (en) * | 2012-10-22 | 2013-01-16 | 天津出入境检验检疫局工业产品安全技术中心 | Melamine detection method |
| CN103920168A (en) * | 2014-03-17 | 2014-07-16 | 上海师范大学 | Nuclear magnetic resonance sensor for detecting melamine based on magnetic nanoparticles, and preparation method and application thereof |
| CN105754036A (en) * | 2016-03-25 | 2016-07-13 | 江南大学 | Preparation method of magnetic molecular imprinting photonic crystal sensor for detecting melamine |
| CN108507854A (en) * | 2018-04-12 | 2018-09-07 | 绿城农科检测技术有限公司 | The pre-treating method of multicomponent agricultural and veterinary chemicals residual quantity in a kind of measurement shellfish samples |
| CN108982787A (en) * | 2018-07-30 | 2018-12-11 | 绿城农科检测技术有限公司 | A method of for detecting melamine in meat |
| US20200246778A1 (en) * | 2019-01-31 | 2020-08-06 | The Governors Of The University Of Alberta | Silica composite monolith as a solid phase extraction material |
-
2019
- 2019-03-08 CN CN201910174962.1A patent/CN109856348A/en active Pending
Patent Citations (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101387609A (en) * | 2008-10-20 | 2009-03-18 | 中国农业大学 | Method for rapidly detecting melamine |
| WO2010090751A2 (en) * | 2009-02-05 | 2010-08-12 | The Regents Of The University Of California | Methods and materials for the detection of melamine |
| CN101576544A (en) * | 2009-04-21 | 2009-11-11 | 新疆出入境检验检疫局检验检疫技术中心 | Method for fast detecting melamine in cream biscuit |
| CN101576543A (en) * | 2009-04-21 | 2009-11-11 | 新疆出入境检验检疫局检验检疫技术中心 | Method for fast detecting melamine in dry milk |
| CN101968452A (en) * | 2010-03-05 | 2011-02-09 | 浙江省疾病预防控制中心 | Kit for quickly detecting tripolycyanamide and use thereof |
| CN102827321A (en) * | 2012-09-06 | 2012-12-19 | 同济大学 | Preparation method and application for magnetic molecularly imprinted polymers for selectively separating carbamazepine |
| CN102879504A (en) * | 2012-10-22 | 2013-01-16 | 天津出入境检验检疫局工业产品安全技术中心 | Melamine detection method |
| CN103920168A (en) * | 2014-03-17 | 2014-07-16 | 上海师范大学 | Nuclear magnetic resonance sensor for detecting melamine based on magnetic nanoparticles, and preparation method and application thereof |
| CN105754036A (en) * | 2016-03-25 | 2016-07-13 | 江南大学 | Preparation method of magnetic molecular imprinting photonic crystal sensor for detecting melamine |
| CN108507854A (en) * | 2018-04-12 | 2018-09-07 | 绿城农科检测技术有限公司 | The pre-treating method of multicomponent agricultural and veterinary chemicals residual quantity in a kind of measurement shellfish samples |
| CN108982787A (en) * | 2018-07-30 | 2018-12-11 | 绿城农科检测技术有限公司 | A method of for detecting melamine in meat |
| US20200246778A1 (en) * | 2019-01-31 | 2020-08-06 | The Governors Of The University Of Alberta | Silica composite monolith as a solid phase extraction material |
Non-Patent Citations (6)
| Title |
|---|
| 周文辉等: "三聚氰胺分子印迹聚合物的制备及奶制品中三聚氰胺的分离", 《分析测试学报》 * |
| 彭涛等: "《中华人民共和国国家标准GB／T22388--2008》", 7 October 2008 * |
| 李保强等: "《壳聚糖生物材料》", 31 December 2017 * |
| 李红梅等: "《中华人民共和国国家标准GB／T22400--2008》", 15 October 2008 * |
| 王露等: "乳制品中三聚氰胺的新型磁性分子印迹聚合物快速萃取法", 《职业与健康》 * |
| 黄华斌等: "分子印迹固相萃取技术－高效液相色谱法测定奶制品和饲料中三聚氰胺含量", 《理化检验(化学分册)》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111521458A (en) * | 2020-04-21 | 2020-08-11 | 深圳市深大检测有限公司 | Method for detecting liquid milk melamine |
| CN111521458B (en) * | 2020-04-21 | 2023-02-03 | 深圳市深大检测有限公司 | Method for detecting liquid milk melamine |
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