CN106645485A - Method for determining content of anionic synthetic pigment in drinks by aminized magnetic nano material - Google Patents
Method for determining content of anionic synthetic pigment in drinks by aminized magnetic nano material Download PDFInfo
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Abstract
The invention relates to a method for determining content of anionic synthetic pigment in drinks by an aminized magnetic nano material. According to the method, the aminized magnetic nano material is taken as a solid-phase extraction adsorbent, electric charges on the surface of the magnetic nano material are changed by regulating pH and are enabled to selectively adsorb the anionic synthetic pigment through electrostatic attraction under the acidic condition, pigment elution is realized through adsorption of the anionic synthetic pigment by electrostatic attraction and repulsion under the alkaline condition, and furthermore, accurate assay determination for the content of the anionic synthetic pigment in drinks is realized in combination with high performance liquid chromatography.
Description
Technical field
The invention belongs to technical field of food safety detection, more particularly to one kind using the magnetic Nano material as admittedly
Phase extractant to determine beverage in anion synthetic dyestuff content method.
Background technology
Color is a notable feature of food, and people add pigment to improve the quality of food generally in food.Color
Element can be divided into natural colouring matter and synthetic dyestuff.Because synthetic dyestuff tinting strength, tinting power is better than natural colouring matter, therefore it is widely used in
In the middle of food.But synthetic dyestuff mostly is the compound containing phenyl ring, xanthene, into after human body, can be metabolized to carcinogenic, cause
Abnormal, mutagenicity aromatic amine compounds, cause damage to health.
At present, the content assaying method of synthetic dyestuff is mainly using solid phase extraction and polycaprolactam method.SPE
Method is cumbersome, expends the time long；Polycaprolactam method, adsorbent is difficult to be completely separated recovery from sample liquid, causes targeted
Compound easily loses during assay.Therefore need to develop a kind of simple to operate, the effect that sample size is determined
The higher method for determining anion synthetic dyestuff content in beverage of rate.
The content of the invention
For the disadvantages described above of prior art, the present invention is provided in a kind of measure beverage using amination magnetic Nano material
The method of anion synthetic dyestuff content.
The technical purpose of the present invention is achieved through the following technical solutions：
The method that utilization amination magnetic Nano material of the present invention determines anion synthetic dyestuff content in beverage,
The step of anion synthetic dyestuff content detection is carried out including the step of carrying out pre-treatment to sample and to the sample after pre-treatment
Suddenly, comprise the following steps wherein carrying out pre-treatment to sample：
1), sample pretreatment：Its pH value is weighed after sample liquid and adjusted to acidity；
2), extract：Add amination magnetic Nano material in the step 1) gained sample liquid in, ultrasound, entered with magnet
Row is separated, abandoning supernatant；
3), drip washing：With step 2 described in acid wash liquid drip washing) gained residue, magnet separate, discard washing lotion；
4), elute：Eluent is added, ultrasound after mixing collects eluent after being separated with magnet, repeat wash-out several times,
Merge eluent, after nitrogen is blown to do, residue ultra-pure water redissolves, to be determined after filtration.
Further, anion synthetic dyestuff assay is carried out to the sample after pre-treatment by high performance liquid chromatography point
Analyse to carry out.
The present invention preferably, when the step 1) in sample when being alcohol in high concentration sample, adjust and heat and go before pH value
Except ethanol.It is highly preferred that the step 1) in pH adjusting agent be formic acid-aqueous solution, pH adjust scope be 2.5～5, preferably
3。
The present invention as it is a kind of preferably, the step 2) described in magnetic Nano material add concentration in sample liquid be 0.2
～1.0mg/ml.More preferably 0.4mg/ml.
The present invention preferably, step 3) described in acid wash liquid be concentration be 0.1～1% formic acid-aqueous solution, preferred concentration
For 0.1%；The step 4) described in eluent be containing concentration for 5%～12% ammoniacal liquor (preferably 10%) methyl alcohol,
Ethanol or acetonitrile solution.Preferably ammoniacal liquor methanol solution.The present invention it is highly preferred that the step 4) in filter adopt polytetrafluoroethyl-ne
Alkene filter membrane is carried out；
The present invention it is highly preferred that the anion synthetic dyestuff selected from famille rose, sunset yellow, red, the carmine 6R of temptation or
One or more materials in crocien orange G.
Specifically, the amination magnetic Nano material is amination magnetic Fe to the present invention3O4Nano material, the material is
Core-shell structure nanometer particle, wherein kernel are magnetic Fe3O4Nano-particle, shell is the organosilane layer with amino-functional group.
Specifically, the amination magnetic Nano material is prepared from the present invention by following steps：
1), magnetic Fe3O4The preparation of nano-particle：Mol ratio is weighed for 1：1～2 FeCl2·4H2O and FeCl3·6H2O
It is dissolved in distilled water and is sufficiently mixed, 80 DEG C～90 DEG C are heated under the protection of nitrogen, dense ammonia is added dropwise under mechanical stirring
Water to solution ph is 10～12, reacts 1～3h；The magnetic Fe_3O_4 nano-particle adsorbing separation that will be generated by magnet, is spent
Ionized water cyclic washing is to solution in neutrality, vacuum drying；
2), magnetic Fe3O4The amination of nano-particle：Weigh step 1) obtained by magnetic Fe3O4Nano-particle, Ran Houjia
Enter absolute ethyl alcohol, deionized water, concentrated ammonia liquor, ultrasonic disperse, mechanical agitation under room temperature is added dropwise Aminosilylation reagent in reactant
In system, 6～12h is fully reacted, using magnet separation product, deionized water cyclic washing, vacuum drying, obtained final product.
The present invention specifically, the step 2) in reactive material adding proportion be：1g magnetic Fes3O4Nano-particle：200～
400ml absolute ethyl alcohols：20～50ml deionized waters：1～5ml concentrated ammonia liquors：200～500 μ l Aminosilylation reagents.
As one kind preferably, it is 3- aminopropyls three that the Aminosilylation reagent is the Aminosilylation reagent to the present invention
Methoxy silane (CAS：13822-56-5), 3- (2- aminoethyls)-aminopropyl trimethoxysilane (CAS：1760-24-3)、N-
Aminoethyl -3- aminopropyl triethoxysilane (CAS：One or more mixing in 5089-72-5), preferably 3- ammonia
Propyl trimethoxy silicane.
Beneficial effects of the present invention：
Compared with existing detection technique, the present invention has following remarkable advantage：
1st, the present invention replaces conventional solid extraction column by the use of new amination magnetic Nano material as solid extracting agent
Or Silon, the efficiency that sample size is determined is improved, reduce the assay cost of sample.Amination magnetic Nano used
Material preparation method is simple, and preparation cost is cheap, and most of laboratory is had ready conditions voluntarily synthetically prepared, and preparation method has
Good GRR, prepared amination magnetic Nano material lot stability is high；In addition, magnetic nano-particle
With magnetic responsiveness and small-size effect, material specific surface area is big, high with pigment joint efficiency, and adsorbent amount is few, and absorption is flat
The weighing apparatus time is short, to reach and only just can need to simply and rapidly realize absorption by using magnet or additional electromagnetic field after adsorption equilibrium
Agent and the separation of solid and liquid of sample liquid, without the need for complex operations such as centrifugation, filtrations, substantially reduce sample size minute, and magnetic point
From thorough, it is difficult to cause damage.
2nd, content assaying method of the present invention is the principle based on Electrostatic Absorption and repulsion, and by adjusting pH amino is changed
Change magnetic Nano material surface institute electrically charged, change absorption property of the material to anion synthetic dyestuff, realize material to pigment
Extraction and desorption.
3rd, the inventive method can simultaneously determine various anion synthetic dyestuffs in beverage, method have good repeatability and
Repeatability, and the method degree of accuracy is high, famille rose, sunset yellow, red, the carmine 6R of temptation, the recovery of standard addition of crocien orange G exist
More than 92%.
Description of the drawings
Fig. 1 is the pre-treatment flow chart of anion synthetic dyestuff in amination magnetic material tests beverage.
Fig. 2 is amination magnetic Fe3O4The SEM electron microscopes of nano material.
Fig. 3 is amination magnetic Fe3O4Zeta potential figure under nano material condition of different pH.
Specific embodiment
In order that the object, technical solutions and advantages of the present invention definitely, are entered below to the preferred embodiments of the present invention
The detailed description of row.
The method that utilization amination magnetic Nano material of the present invention determines anion synthetic dyestuff content in beverage,
The step of anion synthetic dyestuff assay is carried out including the step of carrying out pre-treatment to sample and to the sample after pre-treatment
Suddenly, comprise the following steps wherein carrying out pre-treatment to sample：
1), sample pretreatment：Weigh after sample liquid and adjust its pH value to 2.5～5 with formic acid-aqueous solution, if sample liquid
For alcohol in high concentration sample when, plus adjust pH value after heat abstraction ethanol；
2), extract：Add amination magnetic Nano material in the step 1) gained sample liquid in, ultrasound, carried out with magnet
Quick separating, abandoning supernatant；The magnetic Nano material adds concentration for 0.2～1.0mg/ml in sample liquid
3), drip washing：Formic acid-step 2 described in aqueous solution drip washing with concentration is 0.1～1% (volume fraction)) gained residue
Thing (general drip washing 2 times, the general 3-5ml of consumption, to remove the impurity for remaining in nano-material surface, reduce impurity interference),
Magnet is separated, and discards washing lotion；
4), elute：Eluent is added, ultrasound after being fully vortexed is transferred to eluent in nitrogen blowpipe after being separated with magnet,
Repeat wash-out (test result indicate that the rate of recovery for eluting 3 times just meets requirement) several times, merge eluent, after nitrogen is blown to do,
Residue ultra-pure water redissolves, and Jing after 0.45 μm of teflon membrane filter is filtered efficient liquid phase chromatographic analysis are carried out.Wash-out used
Liquid is containing the methyl alcohol, ethanol or acetonitrile solution that concentration is 5%～12% ammoniacal liquor.
Amination magnetic Nano material of the present invention is amination magnetic Fe3O4Nano material, the material is core shell structure
Nano-particle, wherein kernel are magnetic Fe3O4Nano-particle, shell is the organosilane layer with amino-functional group.
Specifically, the amination magnetic Nano material is prepared from the present invention by following steps：
1), magnetic Fe3O4The preparation of nano-particle：Mol ratio is weighed for 1：1～2 FeCl2·4H2O and FeCl3·6H2O
It is dissolved in distilled water and is sufficiently mixed, 80 DEG C～90 DEG C are heated under the protection of nitrogen, stirs in the machinery of 400rmp～600rmp
It is 10～12 to mix down and be added dropwise over concentrated ammonia liquor to solution ph, reacts 1～3h；The magnetic Fe_3O_4 nanometer that will be generated by magnet
Particle absorption is separated, deionized water cyclic washing to solution in neutrality, then with the moisture in ethanol cyclic washing substitutional solution,
It is vacuum dried at 50 DEG C～60 DEG C；
2), magnetic Fe3O4The amination of nano-particle：Weigh step 1) obtained by magnetic Fe3O4Nano-particle, Ran Houjia
Enter absolute ethyl alcohol, deionized water, concentrated ammonia liquor, ultrasonic disperse, mechanical agitation under room temperature is added dropwise Aminosilylation reagent in reactant
In system, 6～12h is fully reacted, using magnet separation product, deionized water cyclic washing, vacuum is done at 50 DEG C～60 DEG C
It is dry, obtain final product.The reactive material adding proportion is specially：1g magnetic Fes3O4Nano-particle：200～400ml absolute ethyl alcohols：20～
50ml deionized waters：1～5ml concentrated ammonia liquors：200～500 μ l Aminosilylation reagents.
Aminosilylation reagent of the present invention is 3- aminopropyl trimethoxysilanes, 3- (2- aminoethyls)-aminopropyl three
One or more mixing in methoxy silane, N- aminoethyl -3- aminopropyl triethoxysilanes.
Embodiment 1：The preparation method of amination magnetic Nano material
The preparation method of amination magnetic Nano material of the present invention is comprised the following steps：
1), magnetic Fe3O4The preparation of nano-particle：Using chemical coprecipitation, the FeCl of 4.9g is weighed2·4H2O and
The FeCl of 6.7g3·6H2O is dissolved in 100ml distilled water, is transferred in three-neck flask and opens stirring, heats under the protection of nitrogen
To 80 DEG C, under the mechanical agitation of 400rmp～600rmp, be dropwise added dropwise concentration be 1.4mol/L concentrated ammonia liquors until pH value of solution=
10.Subsequently, 3h is stirred under nitrogen protection；After reaction terminates, magnetic Fe will be generated by magnet3O4Nano-particle adsorbing separation,
Deionized water cyclic washing, in neutrality, then wash with ethanol repeatedly to solution, and vacuum drying, obtains final product at 50 DEG C.
2), magnetic Fe3O4The amination of nano-particle：Weigh step 1) prepared by drying 1.0g magnetic Fes3O4Nanometer
Particle adds 200ml absolute ethyl alcohols, 20ml deionized waters and 2ml concentrated ammonia liquors in 500ml three-neck flasks, ultrasonic disperse 30min,
The 3- aminopropyl trimethoxysilanes that 400 μ l are added dropwise under room temperature under mechanical agitation react 6h in reaction system, fully, profit
Use magnet separation product, deionized water cyclic washing then to use ethanol cyclic washing, obtain final product after being vacuum dried at 50 DEG C.
Embodiment 2：The characterizing method of amination magnetic Nano material of the present invention
To embodiment 1 prepare amination magnetic Nano material, respectively using Hitachi S-4800 cold field emission ESEMs,
The full-automatic elemental analyser of Italian Euro Vector EA3000, U.S.'s Quantum Design MPMS3 magnetic measurement systems
Type, the ZetaPALS Zeta potential analyzers of BIC Corp. of the U.S., carry out projection electronic microscope photos, CNH constituent content analysis, and survey
Fixed its Zeta potential at various ph values.
Fig. 2 is the SEM patterns of amination magnetic Nano material prepared by embodiment 1：Show the magnetic Nano material for preparing
In typical sphere, even particle size distribution, particle size meets the size characteristic of nano-particle in 100nm or so.
Table 1 is parallel pair of sample of amination magnetic Nano material prepared by embodiment 1, and with same procedure not same date system
Standby parallel pair of sample of amination magnetic Nano material, by the analysis result of CHN elements in determination of elemental analysis material, as a result shows
Show in 4 parts of prepared magnetic Nano material samples and contain N element, illustrate the magnetic Fe for synthesizing3O4Nanoparticle surface success
N element content is close in silylating reagent containing amino in grafting, and 4 parts of samples, illustrates that the preparation method of the present invention is ripe
Feasible, method has good GRR, and prepared amination magnetic Nano material lot stability is high.
The amination magnetic Nano material of table 1 in a few days Duplicate Samples and the analysis result of the CHN elements of Duplicate Samples in the daytime
| Sample | N (%) | C (%) | H (%) |
| In a few days Duplicate Samples are 1. | 0.281 | 1.288 | 0.379 |
| In a few days Duplicate Samples are 2. | 0.272 | 1.182 | 0.354 |
| In the daytime Duplicate Samples are 1. | 0.282 | 1.452 | 0.381 |
| In the daytime Duplicate Samples are 2. | 0.288 | 1.199 | 0.345 |
Fig. 3 is amination magnetic Nano material Zeta potential at various ph values prepared by embodiment 1, illustrate preparation
In acid condition surface diminishing and increasing amination magnetic Nano material in electropositivity, and electropositive intensity with pH value, works as pH
When value is more than or equal to 7, material surface is in electroneutral or light current negativity.Therefore, the material in acid condition, is inhaled by electrostatic
The effect drawn, will in acid condition show anion synthetic dyestuff (acidic dye) absorption, the enrichment of electronegativity, and in alkaline bar
The wash-out of pigment is realized under part by electrostatic repulsion.
Embodiment 3：Famille rose, sunset yellow, the red, rouge of temptation in amination magnetic Nano material detection mark-on functional beverage
The red 6R of fat, the content of crocien orange G
Detection is comprised the following steps that：
1). the preparation of mark-on functional beverage sample：Add in the commercially available functional beverage without any food colour
Concentration is famille rose, sunset yellow, red, the carmine 6R of temptation, the crocien orange G mixed standard solutions of 1mg/ml, and spiked levels are distinguished
For 0.1 μ g/ml and 1 μ g/ml.
2). extraction：Mark-on sample 25.0ml is taken, with formic acid-aqueous solution (volume ratio 1：2) pH value is adjusted to 3, add and implement
Amination magnetic Nano material 10mg prepared by example 1, quick separating, abandoning supernatant are carried out after ultrasonic 10min with magnet.
3). drip washing：Residue 2 times is washed with 1% formic acid-aqueous solution 3ml, magnet is separated, and discards washing lotion.
4). wash-out：The 10% of 3ml ammonia water-methanol solution is added, ultrasound 1min after being fully vortexed will after magnet separation
Eluent is transferred in 10ml nitrogen blowpipes, repeats wash-out 3 times, merges eluent, and after nitrogen is blown to do, residue is multiple with 2ml ultra-pure waters
It is molten, anion secondary colour in carrying out efficient liquid phase chromatographic analysis to determine beverage Jing after 0.45 μm of teflon membrane filter is filtered
The content of element.
The sample of different spiked levels carries out parallel test, calculates the relative standard deviation between Duplicate Samples, testing result
Such as table 2.
5 kinds of pigment recovery experimental results in the different spiked levels functional beverages of table 2.
Embodiment 4 detects sunset yellow in beverage quality-control sample, carmine content based on amination magnetic Nano material
Based on amination magnetic Nano material detect sunset yellow in beverage quality-control sample, carmine content method such as
Under：
1. extract：5ml samples are drawn, is diluted with 20ml deionized waters, with formic acid-aqueous solution (volume ratio 1:2) adjust and carry
Liquid pH value is taken to 4, the amination magnetic Nano material 15mg for adding embodiment 1 to prepare, is carried out quickly with magnet after ultrasonic 10min
Separate, discard waste liquid.
2. drip washing：Residue 2 times is washed with 1% formic acid-aqueous solution 3ml, magnet is separated, and discards washing lotion.
3. elute：The 8% of 3ml ammonia water-methanol solution, ultrasound 1min after being fully vortexed, magnet is added to wash after separating
De- liquid is transferred in 10ml nitrogen blowpipes, repeats wash-out 3 times, merges eluent, and after nitrogen is blown to do, residue 2ml ultra-pure waters redissolve,
Efficient liquid phase chromatographic analysis, testing result such as table 3 are carried out Jing after 0.45 μm of teflon membrane filter is filtered.
The beverage quality-control sample sunset yellow of table 3, carmine testing result
| Detection project | Standard value (mg/L) | Standard deviation (mg/L) | Test value (mg/L) | Evaluation of result |
| Sunset yellow | 18.7 | 0.2 | 18.5 | It is satisfied |
| It is carmine | 19.6 | 0.2 | 19.2 | It is satisfied |
Remarks：Test result is evaluated using " Z- is than fraction ", is calculated according to Z=(test value-standard value)/standard deviation, works as ︱
Test result satisfaction during Z ︱≤2；When 2<︱ Z ︱<Test result is problematic when 3；When ︱ Z ︱ >=3, test result is unsatisfied with.
Obviously, the above embodiment of the present invention is only intended to clearly illustrate example of the present invention, and is not right
The restriction of embodiments of the present invention.For those of ordinary skill in the field, may be used also on the basis of the above description
To make other changes in different forms.Here all of embodiment cannot be exhaustive.It is every to belong to this
Obvious change that bright technical scheme is extended out changes row still in protection scope of the present invention.
Claims (10)
1. a kind of method that utilization amination magnetic Nano material determines anion synthetic dyestuff content in beverage, including to sample
The step of carrying out pre-treatment and the step of carry out anion synthetic dyestuff assay to the sample after pre-treatment, its feature exists
In carrying out pre-treatment to sample and comprise the following steps：
1), sample pretreatment：Its pH value is weighed after sample liquid and adjusted to acidity；
2), extract：Add amination magnetic Nano material in step 1) gained sample liquid in, ultrasound, then separated with magnet,
Abandoning supernatant；
3), drip washing：With step 2 described in acid wash liquid drip washing) gained residue, magnet separate, discard washing lotion；
4), elute：Eluent is added, ultrasound after mixing collects eluent after being separated with magnet, repeat wash-out several times, merges
Eluent, after nitrogen is blown to do, residue ultra-pure water redissolves, stand-by after filtration.
2. utilization amination magnetic Nano material according to claim 1 determines anion synthetic dyestuff content in beverage
Method, it is characterised in that anion synthetic dyestuff assay is carried out to the sample after pre-treatment by high performance liquid chromatography point
Analyse to carry out.
3. utilization amination magnetic Nano material according to claim 1 determines anion synthetic dyestuff content in beverage
Method, it is characterised in that when the step 1) in sample be alcohol in high concentration sample when, adjust pH value before plus heat abstraction second
Alcohol；Preferably, the step 1) in pH adjusting agent be formic acid-aqueous solution, pH adjust scope be 2.5～5.
4. utilization amination magnetic Nano material according to claim 1 determines anion synthetic dyestuff content in beverage
Method, it is characterised in that the step 2) described in magnetic Nano material add concentration in sample liquid for 0.2～1.0mg/ml.
5. utilization amination magnetic Nano material according to claim 1 determines anion synthetic dyestuff content in beverage
Method, it is characterised in that step 3) described in acid wash liquid be concentration be 0.1～1% formic acid-aqueous solution；The step 4) in
Described eluent is containing the methyl alcohol, ethanol or acetonitrile solution that concentration is 5%～12% ammoniacal liquor；Preferably, the step 4)
Middle filtration is carried out using teflon membrane filter.
6. utilization amination magnetic Nano material according to claim 1 determines anion synthetic dyestuff content in beverage
Method, it is characterised in that the anion synthetic dyestuff is selected from famille rose, sunset yellow, red, the carmine 6R or crocien orange G of temptation
In one or more materials.
7. the utilization amination magnetic Nano material according to any one in claim 1～6 determines anion in beverage
The method of synthetic dyestuff content, it is characterised in that the amination magnetic Nano material is amination magnetic Fe3O4Nano material,
The material is core-shell structure nanometer particle, and wherein kernel is magnetic Fe3O4Nano-particle, shell is having with amino-functional group
Machine silylation layer.
8. the utilization amination magnetic Nano material according to any one in claim 1～6 determines anion in beverage
The method of synthetic dyestuff content, it is characterised in that the amination magnetic Nano material is prepared from by following steps：
1), magnetic Fe3O4The preparation of nano-particle：Mol ratio is weighed for 1：1～2 FeCl2·4H2O and FeCl3·6H2O is dissolved in
It is sufficiently mixed in distilled water, 80 DEG C～90 DEG C is heated under the protection of nitrogen, concentrated ammonia liquor is added dropwise under mechanical stirring extremely
Solution ph is 10～12, reacts 1～3h；The magnetic Fe_3O_4 nano-particle adsorbing separation that will be generated by magnet, uses deionization
Water cyclic washing is to solution in neutrality, vacuum drying；
2), magnetic Fe3O4The amination of nano-particle：Weigh step 1) obtained by magnetic Fe3O4Nano-particle, is subsequently adding anhydrous
Ethanol, deionized water, concentrated ammonia liquor, ultrasonic disperse, mechanical agitation under room temperature, be added dropwise Aminosilylation reagent in reaction system,
Fully 6～12h of reaction, using magnet separation product, deionized water cyclic washing, vacuum drying, obtains final product.
9. utilization amination magnetic Nano material according to claim 8 determines anion synthetic dyestuff content in beverage
Method, it is characterised in that the step 2) in reactive material adding proportion be：1g magnetic Fes3O4Nano-particle：200～400ml
Absolute ethyl alcohol：20～50ml deionized waters：1～5ml concentrated ammonia liquors：200～500 μ l Aminosilylation reagents.
10. utilization amination magnetic Nano material according to claim 8 determines anion synthetic dyestuff content in beverage
Method, it is characterised in that the Aminosilylation reagent be 3- aminopropyl trimethoxysilanes, 3- (2- aminoethyls)-ammonia third
One or more mixing in base trimethoxy silane, N- aminoethyl -3- aminopropyl triethoxysilanes.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611227542.8A CN106645485A (en) | 2016-12-27 | 2016-12-27 | Method for determining content of anionic synthetic pigment in drinks by aminized magnetic nano material |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611227542.8A CN106645485A (en) | 2016-12-27 | 2016-12-27 | Method for determining content of anionic synthetic pigment in drinks by aminized magnetic nano material |
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