CN102998305A - Method for detecting melamine in raw milk by utilizing chromogenic reaction - Google Patents
Method for detecting melamine in raw milk by utilizing chromogenic reaction Download PDFInfo
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Abstract
The invention relates to a method for detecting melamine in raw milk by utilizing a chromogenic reaction. The method comprises two steps of: pre-treating the raw milk by using a protein precipitator and a melamine extracting agent to obtain a melamine pure liquid, putting the pure liquid on a color plate and testing the content of melamine in the raw milk qualitatively or quantitatively by using the chromogenic reaction. The detecting method disclosed by the invention has the advantages of simple conditions, equipment availability, good recovery rate, strong practicability and an exact result, and is a low-cost detecting method.
Description
Technical field
The present invention relates to a kind of detection method of melamine, relate in particular to the detection method of melamine in a kind of raw milk, belong to the analytical chemistry field.
Background technology
Melamine (melamine) is a kind of important azacyclo-Organic Chemicals, has certain renal toxicity.Owing to contain a large amount of ammonia nitrogens in the melamine molecule, nitrogen content reaches 66%, more than four times of protein nitrogen content, has simultaneously preferably stability, in former emulsion process, be difficult to decompose, and there is no the conventional analysis means and detect its existence, so the only a few lawless person adds melamine powder to obtain false protein content in raw milk, cause the melamine pollution in the raw milk to remain in the former emulsion.
The conventional sense method of melamine residual amount has two kinds, a kind of is stratographic analysis, such as high performance liquid chromatography (HPLC), liquid chromatography/mass spectrometry method (LC/MS), Liquid Chromatography-Tandem Mass Spectrometry method (LC/MSMS), this method is had relatively high expectations to sample and testing staff's technical ability, sample pre-treatments and purification process much time power; Another kind method is immunological method, and such as enzyme linked immunosorbent assay (ELISA), this method is long detection time, and expense is higher.
The at present patented claim research about the melamine detection method has a lot, be a kind of enzyme linked immunological kit and method that detects melamine of 200810202732.3 such as number of patent application, number of patent application is 200910060513.0 a kind of melamine colloidal gold immunochromatographydetection detection test paper and preparation method, number of patent application is ELISA kit and the method thereof of a kind of fast detecting content of melamine of 200910061638.5, number of patent application is a kind of melamine hapten of 200910085644.4 and antigen and preparation method thereof and application, number of patent application is 200910107544.7 a kind of fast detection reagent kit for melamine and detection method thereof, and the patent No. provides a kind of detection and quantivative approach of melamine for the patent of US20110069308A1.
Summary of the invention
The invention provides a kind of method of utilizing chromogenic reaction to detect melamine in the raw milk.It is simple that described detection method has condition, and equipment is easy to get, and the recovery is good, practical, and the result is advantage accurately, is a kind of low-cost method that detects.
Detection method of the present invention comprises following two steps: use protein precipitant, melamine extraction agent that raw milk is carried out pre-service and obtain melamine refined solution and refined solution and use content of melamine in the qualitative or former emulsion of quantitative measurement of chromogenic reaction at colour plate.
Described use protein precipitant, melamine extractant carry out the method that pre-service obtains the melamine refined solution to raw milk: the raw milk that adds certain volume in color comparison tube, the albumen precipitation, the melamine extraction agent that add again certain volume, mix, sonic oscillation, centrifugal, then draw supernatant liquor with syringe, be extracted liquid, extract is transferred in the Zeo-karb solid-phase extraction column that activated with 3mL methyl alcohol and 3mL water.Use successively the 0.1mol/L hydrochloric acid of 3mL and the methanol wash of 3mL, be evacuated near doing.Use the eluent wash-out, make refined solution.
Described protein precipitant, melamine extractant are trichloroacetic acid or acetonitrile, and trichloroacetic acid or acetonitrile all are good protein precipitant and melamine extraction agents.Preferred acetonitrile is as protein precipitant and melamine extractant, and this mainly is because find that by the contrast of trichloroacetic acid and acetonitrile corrosivity and the smell of acetonitrile are all less.
Except the key components such as carbohydrates, protein, fat, also have some micro constitutents in the former emulsion, such as nucleotide, vitamins, mineral matter etc., wherein some component can be extracted by acetonitrile solution.Therefore need to the extract after the precipitation be further purified, separate possible interfering material.
Described Zeo-karb solid-phase extraction column is hydrophilic-lipophilic mixed type strong cation exchange solid-phase extraction column, the cationic functional group of strong cation exchange solid-phase extraction column is generally the benzene sulfonic acid base, belong to the strong cation exchange functional group, under any pH condition, all be electronegative negative ion, therefore as long as the pH of Quality control solution makes melamine be the kation state, just can be adsorbed by ion-exchange method by the benzene sulfonic acid base, therefore select the strong cation exchange solid-phase extraction column to get final product, the preferred special-purpose strong cation-exchanging resin of alkaloid that extracts, particularly the C008 of Xi-an Electric Power Resin Factory's production or C004 alkaloid extract resin dedicated.
Described eluent uses methyl alcohol-5% ammonia spirit, also is known as 5% ammoniacal liquor methanol solution.
The preparation of described colour plate: silica gel plate is used the kapillary point sample at 105 ℃ of lower activation 30min, after the drying silica gel plate is put into the chlorine gas environment certain hour, developer is sprayed on the silica gel plate develops the color.
The principle of the content of melamine in the quantitative or former emulsion of qualitative determination of described use chromogenic reaction is: melamine can generate the chloro melamine with chlorine reaction, chloro melamine and potassium iodide reaction can generate iodine, and it is brown that iodine can make starch show.
The method of the content of melamine in the former emulsion of described use chromogenic reaction quantitative measurement is: with the integral optical density of thin layer chromatogram scanner scanning each point, according to the relationship between quality of integral optical density (IOD) with melamine melamine is quantitatively detected.
The method of the content of melamine in the former emulsion of described use chromogenic reaction quantitative measurement can also for: scan silica gel plate with flat bed scanner, obtain scanned picture.Process picture with image processing software, the integral optical density of statistics each point quantitatively detects melamine according to the relationship between quality of integral optical density (IOD) with melamine.
It is further characterized in that:
The consumption of protein precipitant, melamine extractant:
Described protein precipitant and melamine extractant are acetonitrile.Present patent application has been carried out the consumption of protein precipitant, melamine extractant for the research of effect of extracting, in being the former samples of latex of 10mL of 100mg/L, content of melamine adds respectively 10mL, 15mL, 20mL, 25mL acetonitrile, ultrasonic 5min, the centrifugal 5min of 4000r/min, then extract upper layer of extraction liquid with syringe, be settled to 20mL with acetonitrile, adjust pH is 5.Measure the ultra-violet absorption spectrum of extract as shown in Figure 1.When found that the acetonitrile addition is between 15mL～25mL, the melamine effect of extracting is basically identical near the 250nm, but near the impurity percentage extraction the 270nm increases gradually.Therefore described described protein precipitant and melamine extractant are that the addition of acetonitrile is the former emulsion of 15mL～25mL/10mL, and particularly preferred, the addition of acetonitrile is the former emulsion of 15mL/10mL, and namely the volume ratio of acetonitrile and former samples of latex is 1.5: 1.
The selection of liquid and preparation method thereof to be purified:
High performance liquid chromatography and liquid chromatography-mass spectrography all are to adopt the centrifuged supernatant Filter paper filtering to make liquid to be clean.Liquid to be clean passes through solid-phase extraction column, excessively behind the 0.2 μ m organic phase miillpore filter, for HPLC or LC-MS.GC-MS(gas chromatography-mass spectrography) adopts centrifuged supernatant to cross behind the solid-phase extraction column with 0.2 μ m organic phase filtering with microporous membrane.
The fundamental purpose of using miillpore filter in the experiment is the protection chromatographic column, and experiment is found to use syringe to extract centrifuged supernatant and can be obtained settled solution in addition, increases filtering with microporous membrane solution clarification degree is had no significant effect.Present patent application is considered from cost and time angle, adopts syringe to extract centrifuged supernatant, and experiment finds that the centrifugal 5min of 4000r/min just can obtain settled solution.
The condition of solid-phase extraction column:
Get refined solution 3ml is added in the cation exchange solid-phase extraction column (the C008 alkaloid that Xi-an Electric Power Resin Factory produces extracts resin dedicated 4ml) that has activated with the first alcohol and water at every turn, measure the ultraviolet-visible absorption spectroscopy of the rear solution of absorption, reference is 60% acetonitrile solution.Experiment finds that curve shows that without significant change resin does not reach the beginning leakage quantity when filtrate reaches 30ml, and namely exchanging equivalent meets the requirements.
Get the 3ml eluent at every turn and be added to wash-out melamine in the cation exchange solid-phase extraction column, do reference with methyl alcohol and measure absorption spectrum, until curve is steady, obtain the ultraviolet spectrogram such as Fig. 2.Can be found that by Fig. 2 absorption curve is substantially steady when the eluent consumption reaches 9ml, show that melamine is substantially by wash-out.
The selection of color development system:
Melamine behind the wash-out uses chromogenic reaction to detect.The oxidation product of present patent application selection melamine and chlorine and the chromogenic reaction of KI are as coloring reaction system.
The principle of chromogenic reaction is as follows:
This reaction has good color developing, only has melamine to generate brown product in the eluant component, is fit to detect.But because and the chlorine reaction process can't realize liquid phase reactor, therefore at first with melamine eluent point sample in silica gel plate, after the oven dry and chlorine reaction, select iodamylum reagent to do chromogenic reaction.
Description of drawings
Fig. 1 is that content of melamine is the ultraviolet spectrogram of the extract of 100mg/L, and curve 1,2,3,4 acetonitrile add volume and be respectively 10mL, 15mL, 20mL, 25mL.
Fig. 2 is the ultraviolet spectrogram of 100mg/L melamine eluent, and curve 1,2,3 eluant, eluent volumes are respectively 3mL, 6mL, 9mL.
Fig. 3 is the formulation that concerns according to the quality of melamine and integral optical density (IOD), and take melamine concentration as horizontal ordinate, integral optical density is the typical curve that ordinate obtains.
Embodiment
The present invention is described further below in conjunction with embodiment:
The research of embodiment 1, inventive method accuracy
Get 6 cuvettes, respectively successively to the raw milk that wherein adds 10mL25mg/L, 37.5mg/L, 50mg/L, 75mg/L, 100mg/L, 250mg/L, add respectively the 15mL acetonitrile afterwards in 6 cuvettes, concussion mixes, ultrasonic concussion 5min.Then transfer to the centrifugal 5min of 4000r/min in the centrifuge tube, draw supernatant with syringe, adjust pH=3～5, supernatant is transferred in the cation exchange solid-phase extraction column (C008 resin 4mL) that activates with 6mL methyl alcohol and 6mL water, use successively 6mL 0.1mol/L hydrochloric acid and 6mL methanol wash, after being evacuated near doing, with 6mL5% ammoniacal liquor methanol solution wash-out, make refined solution.Get refined solution 2 μ L points to activated good silica gel plate, dry up, again silica gel plate is put into 10min in the environment that is full of chlorine (50mL liquor potassic permanganate and the mixing of 30mL hydrochloric acid solution, 40 ℃).Then with the developer spraying, brown spot occurs, scan silica gel plate with flat bed scanner again, and process picture with Image-pro Plus software.
The formulation that concerns according to the quality of melamine and integral optical density (IOD), take melamine concentration as horizontal ordinate, integral optical density is that ordinate obtains its typical curve as shown in Figure 3, the equation of typical curve is Y=2.6874X+19.744 (r=0.994) (quantitative sensing range 25-250mg/L, method detectability 10mg/L), illustrate that detection method of the present invention can accurately carry out the detection of melamine in the raw milk.
The research of embodiment 2, inventive method precision
Add respectively 10mL50mg/L raw milk and 15mL acetonitrile in color comparison tube, concussion mixes, ultrasonic concussion 5min.Then transfer to the centrifugal 5min of 4000r/min in the centrifuge tube, draw supernatant with syringe, adjust pH=3～5, supernatant is transferred in the cation exchange solid-phase extraction column (C008 resin 4mL) that activates with 6mL methyl alcohol and 6mL water, use successively 6mL 0.1mol/L hydrochloric acid and 6mL methanol wash, after being evacuated near doing, with 6mL5% ammoniacal liquor methanol solution wash-out, make refined solution.Get refined solution 2 μ L points to activated good silica gel plate, dry up, again silica gel plate is put into 10min in the environment that is full of chlorine (50mL liquor potassic permanganate and the mixing of 30mL hydrochloric acid solution, 40 ℃).Then with the developer spraying, brown spot occurs, scan silica gel plate with flat bed scanner again, and process picture with Image-pro Plus software.
Carry out successively 3 parallel laboratory tests, actual measurement IOD is respectively 514.8,514.5,513.9, average IOD514.4, and standard deviation s is 0.46, relative standard deviation RSD is 0.9%.Illustrate that the method for utilizing chromogenic reaction to detect melamine in the raw milk of the present invention has very high precision.
The research of embodiment 3, the inventive method recovery
Get 3 cuvettes, respectively successively to the raw milk that wherein adds 10mL20mg/L, 25mg/L, 50mg/L, add respectively the 15mL acetonitrile afterwards in 3 cuvettes, concussion mixes, ultrasonic concussion 5min.Then transfer to the centrifugal 5min of 4000r/min in the centrifuge tube, draw supernatant with syringe, adjust pH=3～5, supernatant is transferred in the cation exchange solid-phase extraction column (C008 resin 4mL) that activates with 6mL methyl alcohol and 6mL water, use successively 6mL 0.1mol/L hydrochloric acid and 6mL methanol wash, after being evacuated near doing, with 6mL ammoniacal liquor methanol solution wash-out, make refined solution.Get refined solution 2 μ L points to activated good silica gel plate, dry up, again silica gel plate is put into 10min in the environment that is full of chlorine (50mL liquor potassic permanganate and the mixing of 30mL hydrochloric acid solution, 40 ℃).Then with the developer spraying, brown spot occurs, scan silica gel plate with flat bed scanner again, and process picture with Image-pro Plus software, and use the typical curve equation theory of computation IOD value among the embodiment 1, the data that obtain are as shown in table 1:
Table 1 contains the raw milk recovery experiment of melamine
Can get the recovery between 94%-110% by table 1, namely the method for utilizing chromogenic reaction to detect melamine in the raw milk of the present invention has the preferably recovery.
Claims (10)
1. a method of utilizing chromogenic reaction to detect melamine in the raw milk is characterized in that described method comprises following two steps: use protein precipitant, melamine extraction agent raw milk to be carried out pre-service obtain the melamine refined solution; Refined solution uses content of melamine in the qualitative or quantitative measurement milk of chromogenic reaction at colour plate.
2. the method for utilizing chromogenic reaction to detect melamine in the raw milk according to claim 1, it is characterized in that described use protein precipitant, melamine extractant carry out the method that pre-service obtains the melamine refined solution to raw milk and be: the raw milk that in color comparison tube, adds certain volume, the albumen precipitation, the melamine extraction agent that add again certain volume, mix, sonic oscillation, centrifugal, then draw supernatant liquor, be extracted liquid, extract is transferred in the Zeo-karb solid-phase extraction column that activated with 3mL methyl alcohol and 3mL water.Use successively the 0.1mol/L hydrochloric acid of 3mL and the methanol wash of 3mL, be evacuated near doing, use the eluent wash-out, make refined solution.
3. the method for utilizing chromogenic reaction to detect melamine in the raw milk according to claim 1 is characterized in that described protein precipitant, melamine extractant are acetonitrile, and the addition of acetonitrile is 15mL～25mL/10mL raw milk.
4. the method for utilizing chromogenic reaction to detect melamine in the raw milk according to claim 1, the method that it is characterized in that described chromogenic reaction is first with silica gel plate activation 30min under 105 ℃, use the kapillary point sample, after the drying silica gel plate is put into the chlorine gas environment certain hour, developer is sprayed on the silica gel plate develops the color.
5. the method for utilizing chromogenic reaction to detect melamine in the raw milk according to claim 1, the method that it is characterized in that the content of melamine in the described use chromogenic reaction quantitative measurement milk is: with the integral optical density of thin layer chromatogram scanner scanning each point, according to the relationship between quality of integral optical density and melamine melamine is quantitatively detected.
6. the method for utilizing chromogenic reaction to detect melamine in the raw milk according to claim 1, the method that it is characterized in that the content of melamine in the described use chromogenic reaction quantitative measurement milk is: scan silica gel plate with flat bed scanner, obtain scanned picture.Process picture with image processing software, the integral optical density of statistics each point quantitatively detects melamine according to the relationship between quality of integral optical density and melamine.
7. use protein precipitant according to claim 2, melamine extractant carry out the method that pre-service obtains the melamine refined solution to raw milk, it is characterized in that adopting syringe to extract centrifuged supernatant.
8. use protein precipitant according to claim 2, melamine extractant carry out the method that pre-service obtains the melamine refined solution to raw milk, it is characterized in that described ultrasonic time is 5min.
9. use protein precipitant according to claim 2, melamine extractant carry out the method that pre-service obtains the melamine refined solution to raw milk, it is characterized in that described centrifugal condition is the centrifugal 5min of 4000r/min.
10. Zeo-karb solid-phase extraction column according to claim 2, it is characterized in that described Zeo-karb solid-phase extraction column is hydrophilic-lipophilic mixed type strong cation exchange solid-phase extraction column, the preferred special-purpose strong cation-exchanging resin of alkaloid that extracts, particularly the C008 of Xi-an Electric Power Resin Factory's production or C004 alkaloid extract resin dedicated.
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| CN106353313A (en) * | 2016-11-09 | 2017-01-25 | 百奥森（江苏）食品安全科技有限公司 | Rapid detection kit for melamine residue in milk product and use method thereof |
| CN106546583A (en) * | 2016-11-09 | 2017-03-29 | 无锡艾科瑞思产品设计与研究有限公司 | A kind of tripolycyanamide Test paper |
| CN108489973A (en) * | 2018-03-07 | 2018-09-04 | 太原理工大学 | The quantitative testing device and its detection method to concentration are realized based on P integrated with scanner |
| 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 |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104280388A (en) * | 2014-09-20 | 2015-01-14 | 中山鼎晟生物科技有限公司 | Kit and method for rapidly detecting melamine |
| CN105548433A (en) * | 2015-12-17 | 2016-05-04 | 浙江出入境检验检疫局检验检疫技术中心 | Method for simultaneous detection of a plurality of content of non-protein nitrogen-containing compounds in milk by liquid chromatography-tandem mass spectrometry |
| CN106353313A (en) * | 2016-11-09 | 2017-01-25 | 百奥森（江苏）食品安全科技有限公司 | Rapid detection kit for melamine residue in milk product and use method thereof |
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| CN108489973A (en) * | 2018-03-07 | 2018-09-04 | 太原理工大学 | The quantitative testing device and its detection method to concentration are realized based on P integrated with scanner |
| 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 |
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Application publication date: 20130327 |