CN102879504A - Melamine detection method - Google Patents
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- CN102879504A CN102879504A CN2012104027343A CN201210402734A CN102879504A CN 102879504 A CN102879504 A CN 102879504A CN 2012104027343 A CN2012104027343 A CN 2012104027343A CN 201210402734 A CN201210402734 A CN 201210402734A CN 102879504 A CN102879504 A CN 102879504A
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Abstract
The invention relates to a melamine detection method including the steps of (1) sample extraction; (2) supernatant purification; (3) concentration by centrifuging; (4) derivatization; and (5) melamine quantitative detection. By the melamine detection method, a great quantity of samples can be treated simultaneously, 24 samples at most can be treated simultaneously, and various samples can be treated simultaneously; methyl alcohol can be recovered, so that environmental pollution is reduced at the utmost, the recovered methyl alcohol can be reused after distillation, and cost is lowered; a vacuum concentrator comprehensively uses centrifugal force, heating and vacuum effect provided by an external vacuum pump for solvent evaporation, and accordingly multiple samples can be treated without cross contamination; a cold trap is capable of effectively capturing most of solvent vapor damaging to the vacuum pump, so that the high-vacuum oil pump is effectively protected; and the vacuum pump enables a system to be in the vacuum state, the boiling point of solvent is decreased, and evaporation rate of the solvent is accelerated.
Description
Technical field
The invention belongs to the product quality detection field, relate in particular to a kind of detection method of melamine.
Technical background
Melamine (Melamine) is called for short triamine, is a kind of triazines nitrogen heterocyclic ring organic compound, and main application is as producing melamine formaldehyde resin.Because the massfraction about 66% of its nitrogen, some illegal manufacturers add in feed in a large number, to improve crude protein content in the product, hydrobiont is edible to contain in vivo enrichment behind the feed of melamine, grievous injury consumer's health and interests, especially children take the food that melamine exceeds standard, and can cause kidney stone.In September, 2008, " Sanlu milk powder case " caused a large amount of children's kidney stones, with Sanlu, Mongolia Ox, Dairy Enterprise headed by the Erie etc. all detects the melamine that exceeds standard in its product, one time caused people's showing great attention to melamine, thereupon, country has cancelled the inspection-free treatment of food commodity.This directly causes the detection limit of melamine to increase.
At present, the method that is used for the detection of melamine mainly adopts the method for GB/T 22388-2008, comprising: high performance liquid chromatography, liquid chromatography-mass spectrography, gas chromatography-mass spectrography etc.In addition, some testing agencies propose to adopt the electrochromatography instrument to detect at present, for example, Chinese patent CN102650627A discloses a kind of method that a kind of pressurization capillary electric chromatogram instrument detects melamine in the aquatic products that the present invention relates to, and step is: 1) sample preparation; 2) sample pretreatment; 3) preparation melamine standard solution; 4) adopt pressurization capillary electric chromatogram to analyze; 5) carry out quantitative test according to its retention time after sample is analyzed after testing, utilize external standard method to carry out quantitative test according to its peak area.For these detection methods, the sensitivity of liquid phase chromatography is lower, and analysis time is longer, makings, LC-MS instrument, although electrochromatography instrument detection sensitivity and resolution are very high, but these several detection methods all need to adopt nitrogen to dry up instrument, can process faster sample although nitrogen dries up instrument processing melamine sample, but, nitrogen dries up instrument once can only process a small amount of sample, has increased detection time, and can't satisfy at present a large amount of test sample needs the simultaneously demand of detection; , directly be dispersed in the surrounding environment without any processing from the organic solvent that in vitro evaporated by nitrogen blowing, these solvents usually are strong acid, highly basic and strong corrosive material.Very easily therefore the experimenter of direct control health problem occurs, and these solvent evaporates also can work the mischief to surrounding environment in air, comprise the deskman, greening on every side etc.Steam can corrode instrument (syringe needle), causes cross pollution; In addition, nitrogen dries up instrument itself in owing to be in this environment for a long time, the phenomenon that is corroded such as also can occur getting rusty very soon, although some nitrogen dries up the design of instrument syringe needle is wrapped one deck PTFE with anticorrosion, but other parts of the afterbody of pin and instrument can't all be wrapped PTFE, not only affect attractive in appearance, performance, and careless slightly when operation, just iron rust etc. can be touched down in the sample, cause sample contamination; Nitrogen dries up troublesome poeration, must have the people to guard always, has increased testing staff's burden; Consume a large amount of nitrogen, increase testing cost.This shows that improvement nitrogen dries up the defective of instrument in melamine detects and is very important.
Technology contents
Can not a large amount of samples of single treatment for what solve that present detection method exists, toxic gas contaminated environment, the technical matters that consumes a large amount of nitrogen.The invention provides following technical scheme: a kind of detection method of melamine, the method comprises the steps:
(1) extraction of sample
Liquid milk, milk powder, sour milk and toffee etc. take by weighing the 5.00g sample in the 50mL color-comparison tube, the trichloroacetic acid solution that adds 30mL concentration 1wt%, more than the vortex vibration 40s, add again 10mL concentration 1wt% trichloroacetic acid solution, ultrasonic extraction is more than 20 minutes, add the lead acetate solution of 2mL, concentration 22g/L, be settled to scale with 1wt% trichloroacetic acid solution; Fully behind the mixing, shift the centrifuge tube of upper strata extract 29-32mL to 50mL, more than the centrifugal 15min of 5000r/min, obtain supernatant to be clean;
Cheese, cream and chocolate etc. take by weighing the 5.00g sample in the 50mL color-comparison tube, dissolve with the 5mL hot water dissolving or under the condition of heating, the trichloroacetic acid solution that adds again 25mL concentration 1wt%, more than the vortex vibration 40s, add again the ultrasonic extraction of 10mL trichloroacetic acid solution more than 20 minutes, add the lead acetate solution of 2mL, concentration 22g/L, be settled to scale with 1wt% trichloroacetic acid solution; Fully behind the mixing, shift the centrifuge tube of upper strata extract 29-32mL to 50mL, more than the centrifugal 15min of 5000r/min, obtain supernatant to be clean;
(2) purification of supernatant
Getting matrix is the mixed type cation exchange solid-phase extraction column of the polystyrene-divinylbenzene superpolymer of benzene sulfonic acid, first successively with 3-4mL methyl alcohol, the activation of 5-6mL water; Pipette the filtrate to be clean of 5mL to solid-phase extraction column.Use 3-5mL water, the drip washing of 3-5mL methyl alcohol, leacheate is sent into retracting device again, takes out the nearly rear ammonification methanol solution wash-out with 3-5mL volume fraction 5% of doing, and collects eluent; Described ammonification methyl alcohol is that the 5mL volumetric molar concentration is 25%～28% ammoniacal liquor and 95mL methyl alcohol, and is for subsequent use behind the mixing;
(3) centrifugal concentrating
(sample size is adjusted to even number with 12-24 part, odd number amount sample can be joined level with the centrifuge tube of sky and be become an even number) eluent that obtains of sample collection puts in the centrifuge tube of traditional vacuum concentrating instrument simultaneously, carry out the traditional vacuum drying, radiation heating sample under vacuum state; And utilizing the cold-trap of traditional vacuum concentrating instrument to catch solvent vapour, cooling is reclaimed, and sends into retracting device;
(4) derivatization
Get above-mentioned dried residue, add excellent pure level pyridine and the 200 μ L derivatization reagents of 600 μ L, mixing is more than 70 ℃ of reaction 40min; Described derivatization reagent is by 99: 1 N of volume ratio, the two trimethyl silicon based trifluoroacetamides (BSTFA) of O-and trimethyl chlorosilane (TMCS), and wherein said derivatization reagent is chromatographically pure.
(5) the quantitative detection of melamine
At first, draw the melamine standard solution, traditional vacuum is concentrated, and derivatization is made into the standardization solution of derivatization, for measuring, and the drawing standard curve;
The sample that step (4) obtains is measured, compared typical curve, namely obtain the content of melamine in the sample.
Described method also comprises the Methanol Recovery step: the recovery liquid of step (2) and (3) being delivered to retracting device is put in the methyl alcohol distilling apparatus, obtains the methyl alcohol of purifying.
Described method comprises that also the methyl alcohol with distillation purifying is sent to the reusable step of described detection method step (2) again.
Adopting method of the present invention to detect melamine has the following advantages:
1, the vacuum action that provides of Vacuum Concentration instrument comprehensive utilization centrifugal force, heating and external vacuum pump is carried out the solvent evaporation, can process simultaneously a plurality of samples and can not cause cross pollution.
2, cold-trap can effectively catch major part to the prejudicial solvent vapour of vacuum pump, the high vacuum oil pump is provided the protection of effect.
3, vacuum pump makes system be in vacuum state, reduces the boiling point of solvent, accelerates the evaporation rate of solvent.
4, adopt method of the present invention can process simultaneously a large amount of samples, maximum can be processed 24 duplicate samples simultaneously, and can process simultaneously several samples.
5, adopt method of the present invention can reclaim methyl alcohol, the reduction environmental pollution of maximum possible, the methyl alcohol of recovery can be reused after distillation is processed, and the recycling rate of waterused of methyl alcohol reaches more than 80%, has reduced cost.
Description of drawings
Accompanying drawing 1 is that melamine derivative GC-MS selects ion massspectrum figure.
Embodiment
The below is described in detail preferred embodiment of the present invention, thereby so that advantages and features of the invention can be easier to be it will be appreciated by those skilled in the art that protection scope of the present invention is made more explicit defining.
The detection method of melamine, the method comprises the steps:
(1) extraction of sample
Liquid milk, milk powder, sour milk and toffee etc. take by weighing the 5.00g sample in the 50mL color-comparison tube, the trichloroacetic acid solution that adds 30mL concentration 1wt%, more than the vortex vibration 40s, add again 10mL concentration 1wt% trichloroacetic acid solution, ultrasonic extraction is more than 20 minutes, add the lead acetate solution of 2mL, concentration 22g/L, be settled to scale with 1wt% trichloroacetic acid solution; Fully behind the mixing, shift the centrifuge tube of upper strata extract 29-32mL to 50mL, more than the centrifugal 15min of 5000r/min, obtain supernatant to be clean;
Cheese, cream and chocolate etc. take by weighing the 5.00g sample in the 50mL color-comparison tube, dissolve with the 5mL hot water dissolving or under the condition of heating, the trichloroacetic acid solution that adds again 25mL concentration 1wt%, more than the vortex vibration 40s, add again the ultrasonic extraction of 10mL trichloroacetic acid solution more than 20 minutes, add the lead acetate solution of 2mL, concentration 22g/L, be settled to scale with 1wt% trichloroacetic acid solution; Fully behind the mixing, shift the centrifuge tube of upper strata extract 29-32mL to 50mL, more than the centrifugal 15min of 5000r/min, obtain supernatant to be clean;
(2) purification of supernatant
Getting matrix is the mixed type cation exchange solid-phase extraction column of the polystyrene-divinylbenzene superpolymer of benzene sulfonic acid, first successively with 3-4mL methyl alcohol, the activation of 5-6mL water; Pipette the filtrate to be clean of 5mL to solid-phase extraction column.Use 3-5mL water, the drip washing of 3-5mL methyl alcohol, leacheate is sent into retracting device again, takes out the nearly rear ammonification methanol solution wash-out with 3-5mL volume fraction 5% of doing, and collects eluent; Described ammonification methyl alcohol is that the 5mL volumetric molar concentration is 25%～28% ammoniacal liquor and 95mL methyl alcohol, and is for subsequent use behind the mixing;
(3) centrifugal concentrating
(sample size is adjusted to even number with 12-24 part, odd number amount sample can be joined level with the centrifuge tube of sky and be become an even number) eluent that obtains of sample collection puts in the centrifuge tube of traditional vacuum concentrating instrument simultaneously, carry out the traditional vacuum drying, radiation heating sample under vacuum state; And utilizing the cold-trap of traditional vacuum concentrating instrument to catch solvent vapour, cooling is reclaimed, and sends into retracting device;
(4) derivatization
Get above-mentioned dried residue, add excellent pure level pyridine and the 200 μ L derivatization reagents of 600 μ L, mixing is more than 70 ℃ of reaction 40min; Described derivatization reagent is by 99: 1 N of volume ratio, the two trimethyl silicon based trifluoroacetamides (BSTFA) of O-and trimethyl chlorosilane (TMCS), and wherein said derivatization reagent is chromatographically pure.
(5) the quantitative detection of melamine
At first, draw the melamine standard solution, traditional vacuum is concentrated, and derivatization is made into the standardization solution of derivatization, for measuring, and the drawing standard curve;
The sample that step (4) obtains is measured, compared typical curve, namely obtain the content of melamine in the sample.
Step (2) and (3) are delivered to the recovery liquid of retracting device and put in the methyl alcohol distilling apparatus, obtain the methyl alcohol of purifying, then, the methyl alcohol of distillation purifying is sent to the reusable step of described detection method step (2) again.Wherein, more than the recovery 85wt% of methyl alcohol, recycling rate of waterused is more than the 80wt%.
Wherein, described traditional vacuum concentrating instrument mainly by: centrifugal main frame, cold-trap, vacuum pump three parts form, this at last a kind of under vacuum state centrifugal sample, thereby solvent is evaporated instrument with concentrated or dry sample.And the cold-trap that passes through ultralow temperature catches solvent.Sample behind the centrifugal concentrating can be used for various qualitative and quantitative analysis easily.The centrifugal concentrating technological incorporation centrifugal, vacuumize and three kinds of factors of heat, be used for the effectively various solvents of evaporation.
Centrifugal: as to produce the centrifugal force of 200-500 * g, prevent the loss of bumping and sample.Dried solute is deposited on the bottom of container fully, is convenient to the fully recovery of sample.
Vacuumize: the evaporation of accelerated solvent in the SpeedVac concentrating instrument.In concentration process, sample is in a kind of environment that is lower than room temperature all the time, can prevent the part inactivation of thermo-responsive sample.In addition, vacuum state can also prevent the oxidation of sample.
Heat: the evaporation rate of accelerating sample.Do not having under the state of heat credit, aqueous solution can be frozen in concentration process, and this equipment adopts the radiation heating technology, the thermal losses when remedying evaporation.Heat radiation is to the effective means of sample heating under the vacuum state.
The preparation method of described titer draws melamine standard reserving solution 1mL in the 100mL volumetric flask, and to scale, this standard solution 1mL is equivalent to 10 μ g melamine standard items, stores the term of validity 3 months in 4 ℃ of refrigerators with methanol constant volume.Melamine standard reserving solution: accurately take by weighing 100mg (being accurate to 0.1mg) melamine standard items in the 100mL volumetric flask, with methanol aqueous solution dissolving and be settled to scale, be mixed with the standard reserving solution that concentration is 1mg/mL, keep in Dark Place in 4 ℃.
The preparation method of described typical curve is specific as follows: accurately draw melamine standard solution 0,0.4,0.8,1.6,4,8,16mL in 7 100mL volumetric flasks, be diluted to scale with methyl alcohol.Respectively get 1mL and dry up derivatization with nitrogen.Be mixed with the standard solution that derivative products concentration is respectively 0,0.05,0.1,0.2,0.5,1,2 μ g/mL.Reactant liquor is measured for GC-MS.Take the standard operation solution concentration as horizontal ordinate, quota ion mass chromatography peak area is ordinate, the drawing standard working curve.Melamine derivative selects ion massspectrum figure referring to accompanying drawing 1.
Wherein, the operation reference conditions of GC-MS:
A) chromatographic column: 5% phenyl dimethyl polysiloxane quartz capillary column, 30m * 0.25mm * 0.25 μ m, or suitable person.
B) flow velocity: 1.0mL/min.
C) temperature programme: 70 ℃ keep 1min, are warming up to 200 ℃ with the speed of 10 ℃/min, keep 10min.
D) transmission line temperature: 280 ℃.
E) injector temperature: 250 ℃.
F) input mode: Splitless injecting samples.
G) sample size: 1 μ L.
H) ionization mode: electron impact ionization (EI).
I) ionizing energy: 70eV.
J) ion source temperature: 230 ℃.
K) scan pattern: select ion scan, qualitative ion m/z 99,171,327,342, quota ion m/z 327.
Specific embodiment:
Further specify the present invention below by embodiment, but the present invention is not limited to this.The raw material that hereinafter uses is commercially available or can easily makes according to techniques well known.
Embodiment one
Get 18 parts in liquid milk sample, respectively take by weighing the 5.00g sample in the 50mL color-comparison tube, the trichloroacetic acid solution that adds 30mL concentration 1wt%, more than the vortex vibration 40s, add again 10mL concentration 1wt% trichloroacetic acid solution, ultrasonic extraction added the lead acetate solution of 2mL, concentration 22g/L more than 20 minutes, was settled to scale with 1wt% trichloroacetic acid solution; Fully behind the mixing, shift the centrifuge tube of upper strata extract 29-32mL to 50mL, more than the centrifugal 15min of 5000r/min, obtain supernatant to be clean; Purify centrifugal concentrating, derivatization, the quantitative detection of melamine through supernatant; 12 hours detection times, Methanol Recovery rate 90%, recycling rate of waterused 85%.
Embodiment two
Resort to trickery to serve oneself 24 parts in gram force sample, respectively take by weighing the 5.00g sample in the 50mL color-comparison tube, dissolve with the 5mL hot water dissolving or under the condition of heating, the trichloroacetic acid solution that adds again 25mL concentration 1wt%, more than the vortex vibration 40s, add again the ultrasonic extraction of 10mL trichloroacetic acid solution more than 20 minutes, add the lead acetate solution of 2mL, concentration 22g/L, be settled to scale with 1wt% trichloroacetic acid solution; Fully behind the mixing, shift the centrifuge tube of upper strata extract 29-32mL to 50mL, more than the centrifugal 15min of 5000r/min, obtain supernatant to be clean; Purify centrifugal concentrating, derivatization, the quantitative detection of melamine through supernatant; 16 hours detection times, Methanol Recovery rate 95%, recycling rate of waterused 90%.
Claims (4)
1. the method that detects of a melamine, the method comprises the steps:
(1) extraction of sample
Liquid milk, milk powder, sour milk and toffee etc. take by weighing the 5.00g sample in the 50mL color-comparison tube, the trichloroacetic acid solution that adds 30mL concentration 1wt%, more than the vortex vibration 40s, add again 10mL concentration 1wt% trichloroacetic acid solution, ultrasonic extraction is more than 20 minutes, add the lead acetate solution of 2mL, concentration 22g/L, be settled to scale with 1wt% trichloroacetic acid solution; Fully behind the mixing, shift the centrifuge tube of upper strata extract 29-32mL to 50mL, more than the centrifugal 15min of 5000r/min, obtain supernatant to be clean;
Cheese, cream and chocolate etc. take by weighing the 5.00g sample in the 50mL color-comparison tube, dissolve with the 5mL hot water dissolving or under the condition of heating, the trichloroacetic acid solution that adds again 25mL concentration 1wt%, more than the vortex vibration 40s, add again the ultrasonic extraction of 10mL trichloroacetic acid solution more than 20 minutes, add the lead acetate solution of 2mL, concentration 22g/L, be settled to scale with 1wt% trichloroacetic acid solution; Fully behind the mixing, shift the centrifuge tube of upper strata extract 29-32mL to 50mL, more than the centrifugal 15min of 5000r/min, obtain supernatant to be clean;
(2) purification of supernatant
Getting matrix is the mixed type cation exchange solid-phase extraction column of the polystyrene-divinylbenzene superpolymer of benzene sulfonic acid, first successively with 3-4mL methyl alcohol, the activation of 5-6mL water; Pipette the filtrate to be clean of 5mL to solid-phase extraction column.Use 3-5mL water, the drip washing of 3-5mL methyl alcohol, leacheate is sent into retracting device again, takes out the nearly rear ammonification methanol solution wash-out with 3-5mL volume fraction 5% of doing, and collects eluent; Described ammonification methyl alcohol is that the 5mL volumetric molar concentration is 25%～28% ammoniacal liquor and 95mL methyl alcohol, and is for subsequent use behind the mixing;
(3) centrifugal concentrating
(sample size is adjusted to even number with 12-24 part, odd number amount sample can be joined level with the centrifuge tube of sky and be become an even number) eluent that obtains of sample collection puts in the centrifuge tube of traditional vacuum concentrating instrument simultaneously, carry out the traditional vacuum drying, radiation heating sample under vacuum state; And utilizing the cold-trap of traditional vacuum concentrating instrument to catch solvent vapour, cooling is reclaimed, and sends into retracting device;
(4) derivatization
Get above-mentioned dried residue, add excellent pure level pyridine and the 200 μ L derivatization reagents of 600 μ L, mixing is more than 70 ℃ of reaction 40min;
(5) the quantitative detection of melamine
At first, draw the melamine standard solution, traditional vacuum is concentrated, and derivatization is made into the standardization solution of derivatization, for measuring, and the drawing standard curve;
The sample that step (4) obtains is measured, compared typical curve, namely obtain the content of melamine in the sample.
2. the method that detects of melamine as claimed in claim 1, it is characterized in that, described derivatization reagent is by 99: 1 N of volume ratio, the two trimethyl silicon based trifluoroacetamides (BSTFA) of O-and trimethyl chlorosilane (TMCS), and wherein said derivatization reagent is chromatographically pure.
3. the method that detects of melamine as claimed in claim 1 or 2 is characterized in that, also comprises the Methanol Recovery step: the recovery liquid of step (2) and (3) being delivered to retracting device is put in the methyl alcohol distilling apparatus, obtains the methyl alcohol of purifying.
4. the method for melamine detection as claimed in claim 3 is characterized in that, comprises that also the methyl alcohol with distillation purifying is sent to the reusable step of described detection method step (2) again.
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| CN106324147A (en) * | 2016-11-02 | 2017-01-11 | 百奥森（江苏）食品安全科技有限公司 | Detection method for melamine in milk powder |
| CN106831472A (en) * | 2017-03-03 | 2017-06-13 | 北京宇极科技发展有限公司 | A kind of DMF salt bearing liquid wastes recovery process and system |
| CN108169343A (en) * | 2016-12-07 | 2018-06-15 | 内蒙古蒙牛乳业（集团）股份有限公司 | The detection method of neotame content in milk-contained drink |
| CN109856348A (en) * | 2019-03-08 | 2019-06-07 | 浙江省食品药品检验研究院 | A kind of method of melamine in quick measurement meat |
| CN112129855A (en) * | 2020-09-23 | 2020-12-25 | 浙江省疾病预防控制中心 | Method for measuring chloroacetic acid concentration in air by gas chromatography and application thereof |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106324147A (en) * | 2016-11-02 | 2017-01-11 | 百奥森（江苏）食品安全科技有限公司 | Detection method for melamine in milk powder |
| CN108169343A (en) * | 2016-12-07 | 2018-06-15 | 内蒙古蒙牛乳业（集团）股份有限公司 | The detection method of neotame content in milk-contained drink |
| CN106831472A (en) * | 2017-03-03 | 2017-06-13 | 北京宇极科技发展有限公司 | A kind of DMF salt bearing liquid wastes recovery process and system |
| CN106831472B (en) * | 2017-03-03 | 2019-03-22 | 北京宇极科技发展有限公司 | A kind of DMF salt bearing liquid wastes recovery process |
| CN109856348A (en) * | 2019-03-08 | 2019-06-07 | 浙江省食品药品检验研究院 | A kind of method of melamine in quick measurement meat |
| CN112129855A (en) * | 2020-09-23 | 2020-12-25 | 浙江省疾病预防控制中心 | Method for measuring chloroacetic acid concentration in air by gas chromatography and application thereof |
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