CN105628669A - Detection method of melamine in milk and milk powder - Google Patents
Detection method of melamine in milk and milk powder Download PDFInfo
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- CN105628669A CN105628669A CN201410591241.8A CN201410591241A CN105628669A CN 105628669 A CN105628669 A CN 105628669A CN 201410591241 A CN201410591241 A CN 201410591241A CN 105628669 A CN105628669 A CN 105628669A
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Abstract
The invention discloses a detection method of melamine in milk and milk powder. Separation and enrichment characteristics of coffee-ring effect and high resolution detection of confocal micro-raman spectroscopy are fully combined, and a new detection method of low-concentration melamine in milk and milk powder is provided. The new detection method is simple and shortcut and has advantages of low cost and accurate result. Only by normal evaporation process, low-cost detection can be realized. The method is beneficial to large-batch low-cost rapid screening. The invention provides a new technical means for detection of melamine in milk and milk powder products.
Description
Technical field
The present invention relates to a kind of detection method, be specifically related in a kind of milk and milk powder the detection method of tripolycyanamide.
Background technology
From " the Sanlu baby milk powder event " of 2008, milk product safety problem was created great concern by people, but the tripolycyanamide event in milk and milk powder still again and again occurs, remains incessant after repeated prohibition. Therefore, in the urgent need to developing simplicity, efficient detection method, to meet tripolycyanamide testing requirement in increasingly serious milk and milk powder product. At present, both at home and abroad about the detection method of tripolycyanamide, mainly there are high performance liquid chromatography (HPLC), gas chromatography, the chromatography of ions, gas chromatography mass spectrometry (GC-MS) and LC-MS (LC-MS) etc., These methods, while the tripolycyanamide that can detect exactly in milk and milk powder product, but all exist complicated operation, sample processing time length, cannot the problems such as rapid screening, detection workload be big and expensive.
Coffee toroidal effect be by Deegan et al. take the lead in propose a kind of separation and concentration new phenomenon, there is the features such as simple, efficient. Coffee toroidal effect is not limited solely to infusion, is also present in multiple solution system widely, and by the separation and concentration of coffee toroidal effect, the sensitivity that can greatly improve subsequent detection is even higher to 1mg/L.
Copolymerization Jiao's micro Raman spectra is a kind of micro-region analysis technique with the advantage such as high-resolution, high flux, the position of its spectrum peak, quantity and strength information directly reflect composition and the Constellation information of molecule, can directly the microcell sample of different shape be tested. By organically combining the accurate detection of the separation and concentration characteristic of coffee toroidal effect and Raman spectrum, can the tripolycyanamide of low concentration in high throughput testing milk and milk powder product, therefore there is very wide application prospect.
Summary of the invention
For solving the problems referred to above, the invention provides the detection method of tripolycyanamide in a kind of milk and milk powder, easy and simple to handle, quickly and result accurate, favorable reproducibility; Can be greatly simplified detecting step, reduce testing cost, the work efficiency improving supervision department, the high flux inspection that realizes milk and milk powder are had great social benefit.
For achieving the above object, the technical scheme that the present invention takes is:
In a kind of milk and milk powder, the detection method of tripolycyanamide, comprises the steps:
S1, prepare the tripolycyanamide storing solution of variable concentrations with distilled water or pure water;
S2, variable concentrations prepared by step S1 tripolycyanamide storing solution be separately added in milk without tripolycyanamide itself or milk powder lysate, fully vibration is uniformly mixed so as to obtain mixed liquor;
S3, the mixed liquor of step S2 gained is mixed in appropriate proportions with dehydrated alcohol, after shaken well, centrifugal obtain upper strata clarification extracting solution;
S4, the clarification extracting solution of step S3 gained is dropped in substrate, after room temprature evaporation, obtain coffee ring;
S5, tripolycyanamide is carried out copolymerization Jiao's micro Raman spectra detection, obtain its Raman spectrum;
S6, to step S4 formed coffee ring material carry out copolymerization Jiao's micro Raman spectra detection, obtain its Raman spectrogram;
The raman spectra position of S7, the raman spectra position of relative analysis coffee ring material and tripolycyanamide, it is judged that exist with or without tripolycyanamide.
The described sampling amount that milk powder lysate is milk powder is 1g, puts into and is settled to 10ml with distilled water or pure water in the beaker of 25ml and magnetic agitation is uniformly mixed so as to obtain lysate.
Melamine concentration respectively 0mg/kg, 1mg/kg, 5mg/kg, 10mg/kg, 50mg/kg, 100mg/kg, 500mg/kg and 1000mg/kg in the mixed liquor configured in described step S2.
In described step S3, dehydrated alcohol used is 99.7%, and described mixed liquor and dehydrated alcohol mixed proportion are 1:2.
Described step S3 can be replaced the mixed liquor acid adding adjustment PH taking step S2 gained and precipitates out to protein denaturation.
Acid used is the hydrochloric acid of 1mol/L for concentration, and regulating PH is 4.7.
Substrate in described step S4 is sheet metal or metal coating glass.
The method have the advantages that
The present invention fully combines the separation and concentration characteristic of coffee toroidal effect and the high resolution detection of copolymerization Jiao's micro Raman spectra, provide a kind of simple and efficient, cost is low and the new detecting method of low concentration tripolycyanamide in result milk accurately and milk powder, only need to can realize low cost detection by normal evaporation process. The method is advantageously implemented the rapid screening of high-volume low cost, provides a kind of new technical means for the detection of tripolycyanamide in milk and milk powder product.
Detailed description of the invention
In order to make objects and advantages of the present invention clearly understand, below in conjunction with embodiment, the present invention is further elaborated. Should be appreciated that specific embodiment described herein is only in order to explain the present invention, is not intended to limit the present invention.
The Cleaning Principle of the present invention is:
Tripolycyanamide has unsaturated bond structure, and Raman signal intensity is big, and feature spectral peak is sharp-pointed, by coffee toroidal effect, it is possible to make the material in milk or milk powder product obtain separation and concentration. Judge the position of test substance on coffee ring by copolymerization Jiao's micro Raman spectra, and measure its Raman spectrum, by with the spectral peak multilevel iudge testing sample of tripolycyanamide standard sample in whether contain tripolycyanamide.
Originally the instrument and equipment being embodied as using is:
Magnetic stirring apparatus, centrifuge, pH meter, copolymerization Jiao's micro-Raman spectroscopy. Adjustable pipette (1-50 �� L, 20-200 �� L, 100-1000 �� L), pipettor head 20-200 �� L and 100-1000 �� L, 25ml beaker, 10ml centrifuge tube.
Agents useful for same is as follows:
(1) tripolycyanamide powder standard substance, commercially available.
(2) dehydrated alcohol, 99.7%, commercially available; Hydrochloric acid, 11.9mol/L, commercially available.
(3) sheet metal, commercially available; Coated glass, self-control.
(4) distilled water or pure water, commercially available.
Embodiment 1
S11, milk treatment process are as follows:
Take respectively 2ml containing variable concentrations tripolycyanamide (1,5,10,50,100,500,1000mg/kg) milk sample in 10ml centrifuge tube, accurately adding dehydrated alcohol 4ml, fully vibration is uniformly mixed so as to obtain mixed liquor. After mixed liquor in centrifuges centrifugal 5min, take upper strata clarification extracting solution.
The detection limit of this method is 1mg/kg.
S12, sample coffee ring preparation
Draw the clarification extracting solution obtained with pipettor, drip in metallic substrates or coated glass substrate, under room temperature condition after evaporation, obtain the coffee ring that testing sample is formed.
S13, coffee ring material copolymerization Jiao's micro Raman spectra detection
The coffee ring formed by the testing sample obtained, is placed under the microscope of copolymerization Jiao's micro-Raman spectroscopy, observes the distribution of coffee ring material, coffee ring material is carried out Raman spectrum detection, obtains the Raman spectrogram of zones of different on coffee ring. Copolymerization Jiao's micro Raman spectra of contrast standard tripolycyanamide sample, finds out tripolycyanamide position on coffee ring according to spectrum peak position, and judges whether tripolycyanamide exists.
Embodiment 2
S21, milk treatment process are as follows:
Take 10ml containing variable concentrations tripolycyanamide (1,5,10,50,100,500,1000mg/kg) milk sample in 25ml beaker. The hydrochloric acid (distilled water or pure water dilution) of preparation 1mol/L, adds appropriate hydrochloric acid in milk sample, regulates PH to 4.7, make protein denaturation precipitate out, and fully vibration is uniformly mixed so as to obtain mixed liquor. Take mixed liquor 5ml and be placed in 10ml centrifuge tube, after centrifuge 5min, take upper strata clarification extracting solution.
The detection limit of this method is 1mg/kg.
S22, sample coffee ring preparation
Draw the clarification extracting solution obtained with pipettor, drip in metallic substrates or coated glass substrate, under room temperature condition after evaporation, obtain the coffee ring that testing sample is formed.
S23, coffee ring material copolymerization Jiao's micro Raman spectra detection
The coffee ring that the testing sample obtained is formed, is placed under the microscope of copolymerization Jiao's micro-Raman spectroscopy, observes the distribution of coffee ring material, coffee ring material is carried out Raman spectrum detection, obtains the Raman spectrogram of zones of different on coffee ring. Copolymerization Jiao's micro Raman spectra of contrast standard tripolycyanamide sample, finds out tripolycyanamide position on coffee ring according to spectrum peak position, and judges whether tripolycyanamide exists.
Embodiment 3
S31, milk powder processing method are as follows:
Taking 1g powdered milk sample to 25ml beaker, accurately add distilled water or pure water 9ml, magnetic agitation obtains lysate. The tripolycyanamide storing solution of variable concentrations is added in lysate so that it is the concentration of middle tripolycyanamide is 1,5,10,50,100,500,1000mg/kg. The hydrochloric acid (distilled water or pure water dilution) of preparation 1mol/L, adds appropriate hydrochloric acid in the milk powder lysate containing tripolycyanamide, regulates PH to 4.7, make protein denaturation precipitate out, and fully vibration is uniformly mixed so as to obtain mixed liquor. Take mixed liquor 5ml and be placed in 10ml centrifuge tube, centrifuge 5min, take upper strata clarification extracting solution.
The detection limit of this method is 1mg/kg.
S32, sample coffee ring preparation
Draw the clarification extracting solution obtained with pipettor, drip in metallic substrates or coated glass substrate, under room temperature condition after evaporation, obtain the coffee ring that testing sample is formed.
S33, coffee ring material copolymerization Jiao's micro Raman spectra detection
The coffee ring that the testing sample obtained is formed, is placed under the microscope of copolymerization Jiao's micro-Raman spectroscopy, observes the distribution of coffee ring material, coffee ring material is carried out Raman spectrum detection, obtains the Raman spectrogram of zones of different on coffee ring. Copolymerization Jiao's micro Raman spectra of contrast standard tripolycyanamide sample, judges tripolycyanamide position on coffee ring according to spectrum peak position, and judges the existence of tripolycyanamide.
In sum, originally the high resolution detection fully combining the separation and concentration characteristic of coffee toroidal effect and copolymerization Jiao's micro Raman spectra it is embodied as, provide a kind of simple and efficient, cost is low and the new detecting method of low concentration tripolycyanamide in result milk accurately and milk powder, only need to can realize low cost detection by normal evaporation process. The method is advantageously implemented the rapid screening of high-volume low cost, provides a kind of new technical means for the detection of tripolycyanamide in milk and milk powder product.
The above is only the preferred embodiment of the present invention; it should be pointed out that, for those skilled in the art, under the premise without departing from the principles of the invention; can also making some improvements and modifications, these improvements and modifications also should be regarded as protection scope of the present invention.
Claims (7)
1. the detection method of tripolycyanamide in a milk and milk powder, it is characterised in that comprise the steps:
S1, prepare the tripolycyanamide storing solution of variable concentrations with distilled water or pure water;
S2, variable concentrations prepared by step S1 tripolycyanamide storing solution be separately added in milk without tripolycyanamide itself or milk powder lysate, fully vibration is uniformly mixed so as to obtain mixed liquor;
S3, the mixed liquor of step S2 gained is mixed in appropriate proportions with dehydrated alcohol, after shaken well, centrifugal obtain upper strata clarification extracting solution;
S4, the clarification extracting solution of step S3 gained is dropped in substrate, after room temprature evaporation, obtain coffee ring;
S5, tripolycyanamide is carried out copolymerization Jiao's micro Raman spectra detection, obtain its Raman spectrum;
S6, to step S4 formed coffee ring material carry out copolymerization Jiao's micro Raman spectra detection, obtain its Raman spectrogram;
The raman spectra position of S7, the raman spectra position of relative analysis coffee ring material and tripolycyanamide, it is judged that exist with or without tripolycyanamide.
2. the detection method of tripolycyanamide in a kind of milk according to claim 1 and milk powder, it is characterized in that, the described sampling amount that milk powder lysate is milk powder is 1g, puts into and is settled to 10ml with distilled water or pure water in the beaker of 25ml and magnetic agitation is uniformly mixed so as to obtain lysate.
3. the detection method of tripolycyanamide in a kind of milk according to claim 1 and milk powder, it is characterized in that, melamine concentration respectively 0mg/kg, 1mg/kg, 5mg/kg, 10mg/kg, 50mg/kg, 100mg/kg, 500mg/kg and 1000mg/kg in the mixed liquor configured in described step S2.
4. the detection method of tripolycyanamide in a kind of milk according to claim 1 and milk powder, it is characterised in that in described step S3, dehydrated alcohol used is 99.7%, and described mixed liquor and dehydrated alcohol mixed proportion are 1:2.
5. the detection method of tripolycyanamide in a kind of milk according to claim 1 and milk powder, it is characterised in that described step S3 can be replaced the mixed liquor acid adding taking step S2 gained and regulates PH and precipitate out to protein denaturation.
6. the detection method of tripolycyanamide in a kind of milk according to claim 5 and milk powder, it is characterised in that acid used is concentration is the hydrochloric acid of 1mol/L, regulating PH is 4.7.
7. the detection method of tripolycyanamide in a kind of milk according to claim 1 and milk powder, it is characterised in that the substrate in described step S4 is sheet metal or metal coating glass.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108760672A (en) * | 2018-05-22 | 2018-11-06 | 深圳市太赫兹科技创新研究院 | The detection method of melamine |
| CN109239049A (en) * | 2018-09-13 | 2019-01-18 | 常州常检诺食品检测中心有限公司 | The detection method of melamine in a kind of milk powder |
| CN114280029A (en) * | 2022-01-04 | 2022-04-05 | 朱媛媛 | Method for detecting western medicine components in Chinese patent medicine |
Citations (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101477051A (en) * | 2008-10-28 | 2009-07-08 | 中国检验检疫科学研究院 | Raman spectrum method and reagent kit used for on-site fast detection of melamine in liquid milk |
| CN101487797A (en) * | 2009-02-24 | 2009-07-22 | 中国检验检疫科学研究院 | Method for measuring melamine content in liquid example |
| CN101672786A (en) * | 2009-03-12 | 2010-03-17 | 中国科学院理化技术研究所 | Active substrate with surface provided with enhanced raman scattering effect and production method and application thereof |
| CN102087217A (en) * | 2011-01-14 | 2011-06-08 | 河北省食品质量监督检验研究院 | Laser Raman spectroscopy method for quickly analyzing content of melamine in milk powder |
| CN102156118A (en) * | 2011-03-22 | 2011-08-17 | 中国科学院长春应用化学研究所 | Method for detecting melamine |
| CN102680306A (en) * | 2012-05-15 | 2012-09-19 | 中国检验检疫科学研究院 | Quick pretreatment method for detecting melamine in raw material milk |
| CN103196890A (en) * | 2013-04-24 | 2013-07-10 | 中国农业科学院农业质量标准与检测技术研究所 | Method for rapidly detecting melamine in forage based on surface enhanced Raman scattering spectrum |
| CN103411950A (en) * | 2013-06-24 | 2013-11-27 | 吉林大学 | Method for detecting tripolycyanamide in milk based on surface-enhanced Raman activity chip |
| CN103529013A (en) * | 2013-10-18 | 2014-01-22 | 福建师范大学 | Method for rapidly detecting seminal plasma fructose based on DCDR spectrum technique |
| CN103604794A (en) * | 2013-11-26 | 2014-02-26 | 厦门大学 | Tear test method based on surface-enhanced raman spectroscopy |
| CN104122246A (en) * | 2013-04-28 | 2014-10-29 | 同方威视技术股份有限公司 | Raman-spectrum measuring method for detecting content of melamine in milk products with different matrixes |
-
2014
- 2014-10-28 CN CN201410591241.8A patent/CN105628669A/en active Pending
Patent Citations (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101477051A (en) * | 2008-10-28 | 2009-07-08 | 中国检验检疫科学研究院 | Raman spectrum method and reagent kit used for on-site fast detection of melamine in liquid milk |
| CN101487797A (en) * | 2009-02-24 | 2009-07-22 | 中国检验检疫科学研究院 | Method for measuring melamine content in liquid example |
| CN101672786A (en) * | 2009-03-12 | 2010-03-17 | 中国科学院理化技术研究所 | Active substrate with surface provided with enhanced raman scattering effect and production method and application thereof |
| CN102087217A (en) * | 2011-01-14 | 2011-06-08 | 河北省食品质量监督检验研究院 | Laser Raman spectroscopy method for quickly analyzing content of melamine in milk powder |
| CN102156118A (en) * | 2011-03-22 | 2011-08-17 | 中国科学院长春应用化学研究所 | Method for detecting melamine |
| CN102680306A (en) * | 2012-05-15 | 2012-09-19 | 中国检验检疫科学研究院 | Quick pretreatment method for detecting melamine in raw material milk |
| CN103196890A (en) * | 2013-04-24 | 2013-07-10 | 中国农业科学院农业质量标准与检测技术研究所 | Method for rapidly detecting melamine in forage based on surface enhanced Raman scattering spectrum |
| CN104122246A (en) * | 2013-04-28 | 2014-10-29 | 同方威视技术股份有限公司 | Raman-spectrum measuring method for detecting content of melamine in milk products with different matrixes |
| CN103411950A (en) * | 2013-06-24 | 2013-11-27 | 吉林大学 | Method for detecting tripolycyanamide in milk based on surface-enhanced Raman activity chip |
| CN103529013A (en) * | 2013-10-18 | 2014-01-22 | 福建师范大学 | Method for rapidly detecting seminal plasma fructose based on DCDR spectrum technique |
| CN103604794A (en) * | 2013-11-26 | 2014-02-26 | 厦门大学 | Tear test method based on surface-enhanced raman spectroscopy |
Non-Patent Citations (4)
| Title |
|---|
| DONGMAO ZHANG等: "Raman Detection of Proteomic Analytes", 《ANALYTICAL CHEMISTRY》 * |
| F. SIAK等: "Raman spectra of drop coating deposition Raman for melamine solution", 《2012 IEEE EMBS CONFERENCE ON BIOMEDICAL ENGINEERING & SCIENCES》 * |
| 胡佩等: "滴涂沉积拉曼光谱技术在泪液分析中的应用", 《第十七届全国光散射学术会议》 * |
| 陈君义等: "食品和饲料中三聚氰胺检测技术研究进展", 《粮油食品科技》 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108760672A (en) * | 2018-05-22 | 2018-11-06 | 深圳市太赫兹科技创新研究院 | The detection method of melamine |
| CN109239049A (en) * | 2018-09-13 | 2019-01-18 | 常州常检诺食品检测中心有限公司 | The detection method of melamine in a kind of milk powder |
| CN114280029A (en) * | 2022-01-04 | 2022-04-05 | 朱媛媛 | Method for detecting western medicine components in Chinese patent medicine |
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