CN104237438B - Tenax makes analogies-GCMS and measures the method for the migration amount of aromatic amine in paper and cardboard - Google Patents
Tenax makes analogies-GCMS and measures the method for the migration amount of aromatic amine in paper and cardboard Download PDFInfo
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Abstract
Disclosure is a kind of measures the method for aromatic amine migration amount in paper and cardboard, adopts the polyphenylene oxide of improvement as analogies, the aromatic amine that analogies migrate through gas chromatography/mass spectrometry after solvent extraction, extract concentration. Step provided by the present invention and method can be effectively used for measuring the migration amount moving to specific aromatic amine in dry food analogies from paper and cardboard, and method is feasible, simple to operate, and method is accurate, highly sensitive, has application value.
Description
Technical field
The present invention relates to and a kind of measure the method for specific aromatic amine migration amount in paper and cardboard, it is specifically related to adopt the polyphenylene oxide (MPPO of improvement, Tenax) as analogies, analogies measure, through GC-MS (GC/MS), the aromatic amine migrated after solvent extraction, extract concentration.
Background technology
Paper wrapper, as the important packaging material of a class, is widely used, and these wrapping papers would generally impressing pattern or word, it is possible to use the coating containing azo dye. Part azo dye can decompose under certain condition and discharges aromatic amine, and many aromatic amines are to health and bad environmental, and especially 2,4-dimethylanilines, 2-naphthylamines, parachloroanilinum, benzidine, 4-aminobphenyl etc. are carcinogen. When paper wrapper directly and Food Contact, the harmful aromatic amine wherein contained may migrate in food, brings high risks to human health, it is therefore necessary to strictly limit its from packaging material to food migration.
Investigating whether harmful aromatic amine migrates, whether the amount of migration reaches to jeopardize the level of human health, and direct investigation mode is exactly detect the contained amount migrating aromatic amine in the food contacted with packaging Paper or cardboard.Owing to being difficult to carry out each food migrating quantifier elimination, namely most efficient method is chosen suitable analogies and is set up migration models, obtains migration amount. But relevant laws and regulations and document there is not yet the migration models by setting up dry food analogies and method both at home and abroad, carry out the research that aromatic amine in paper wrapper moves in dry food.
Using Tenax as the analogies of dry food, in conjunction with gas chromatography/mass spectrometry method, set up the concrete operation step moving to harmful aromatic amine in dry food analogies in mensuration paper and cardboard and method is very meaningful.
Summary of the invention
For filling up the vacancy of prior art, the present invention provides a kind of and measures the method for specific aromatic amine migration amount in paper and cardboard, it is specifically related to adopt the polyphenylene oxide (MPPO of improvement, Tenax) as analogies, analogies are through solvent extraction, and extract measures the aromatic amine migrated through GC-MS (GC/MS).
It is an object of the invention to be achieved through the following technical solutions: a kind of measure the method for aromatic amine migration amount in paper and cardboard, it is characterised in that through following each step:
(1) Paper or cardboard to be measured is cut into 0.2～1.0dm2Sample, be taken as sample to be tested, sample to be tested be laid in container bottom, with Food Contact facing to upper, tile Tenax on sample to be tested surface, then be placed at 5～150 DEG C constant temperature and keep 5min～240h, is cooled to room temperature;
(2) Tenax1.0～5.0g of sample to be tested in step (1) is taken out, it is placed in tool plug triangular flask and carries out extracting to obtain extracting solution for 1:10 addition solvent by solid-to-liquid ratio (g/mL), again by extracting solution in 35 DEG C of nitrogen blow be concentrated into dry, add 2.0mL t-butyl methyl ether dissolve to obtain lysate;
(3) lysate of aspiration step (2), cross 0.22 μm of organic system microporous filter membrane, arranging the ion Selection parameter of specific aromatic amine and internal standard substance, adopt gas chromatography/mass spectrometry method analysis to obtain the quota ion peak area of each aromatic amine and internal standard substance in lysate, instrument condition is as follows:
The condition of gas chromatogram is chromatographic column DB-5 elastic capillary-column [fixing mutually for (50% phenyl)-methyl polysiloxane], 30m (length) × 0.25mm (internal diameter) × 0.25 μm (thickness); Injector temperature: 250 DEG C; Carrier gas: helium (purity >=99.999%); Constant current flow velocity: 1.0mL/min; Sample size: 1 μ L; Split ratio 10:1; Heating schedule: initial temperature 50 DEG C, keep 1min, with 5 DEG C/min to 280 DEG C, keep 8min;
Mass spectrographic condition is ion source: EI source; Ion source temperature: 230 DEG C; Ionizing energy: 70eV; Scan mode: full scan and selection ion scan (SIM); Sweep limits: m/z35～270amu; Solvent delay: 9.0min; Interface temperature: 280 DEG C;
(4) the serial mixed standard solution of 21 kinds of aromatic amines is prepared with t-butyl methyl ether for solvent, series standard solution concentration is 0.5 μ g/mL, 2.5 μ g/mL, 5 μ g/mL, 10 μ g/mL, 25 μ g/mL, it is simultaneously introduced interior mark: naphthalene-d8,2,4,5-trichloroaniline, anthracene-d10, interior mark concentration is 2.5 μ g/mL; Series standard solution is carried out gas chromatograph-mass spectrometer (GC-MS) analysis, in each titer, the peak area of 21 kinds of aromatic amine quota ions and the quota ion peak area ratio at interior mark peak are for vertical coordinate, in each standard working solution, the concentration of 21 kinds of aromatic amines is for abscissa, makes the standard curve of 21 kinds of aromatic amines;
(5) according to step (4) gained standard curve, the quota ion peak area of each aromatic amine and internal standard substance in lysate, substitute into standard curve and calculate the concentration obtaining aromatic amine, in sample to be tested, the migration amount of specific aromatic amine is calculated by formula (1):
... ... ... ... ... ... (1)
In formula:
The migration amount of specific aromatic amine in X sample, unit is microgram every square decimeter (μ g/dm2);
C is drawn the concentration of aromatic amine in lysate by standard curve, and unit is micrograms per millilitre (μ g/mL);
Redissolving the volume of solvent after the concentration of V extracting solution, unit is milliliter (mL).
In described step (1), the tiling amount of Tenax presses every dm2Sample to be tested add 5g.
Described step (1) is placed at 5～100 DEG C constant temperature and keeps time conditions and the temperature conditions of 5min～240h employing table 1 and table 2 to be controlled:
The time conditions of table 1 test
| It is contemplated that the most sternly use when time of contact | Test period |
| t≤5 min | 5 min |
| 5 min≤t≤ 0.5 h | 0.5 h |
| 0.5 h≤t≤ 1 h | 1 h |
| 1 h≤t≤ 2 h | 2 h |
| 2 h≤t≤ 4 h | 4 h |
| 4 h≤t≤ 24 h | 24 h |
| T > 24 h | 240 h |
The temperature conditions of table 2 test
| It is contemplated that the most sternly use when Contact Temperature | Test temperature |
| T≤5 ℃ | 5 ℃ |
| 5 DEG C of < T≤20 DEG C | 20 ℃ |
| 20 DEG C of < T≤40 DEG C | 40 ℃ |
| 40 DEG C of < T≤70 DEG C | 70 ℃ 2 --> |
| 70 DEG C of < T≤100 DEG C | 100 DEG C or reflux temperature |
| 100 DEG C of < T≤121 DEG C | 121 ℃ |
| 121 DEG C of < T≤130 DEG C | 130 ℃ |
| 130 DEG C of < T≤150 DEG C | 150 ℃ |
| T > 150 DEG C | 175 ℃ |
In described step (2), solvent is the ethyl acetate-t-butyl methyl ether solution of 1:1 (v/v).
Extracting in described step (2) is at room temperature mechanical shaking extraction 0.5h.
The specific aromatic amine of described step (3) includes ortho-aminotoluene, 2, 4-dimethylaniline, 2, 6-dimethylaniline, o-aminoanisole, parachloroanilinum, 2, 4, 5-trimethylaniline, 2-methoxyl group-5-monomethylaniline., 4-chloro-o-toluidine, 2, 4-diaminotoluene, 2, 4-diamino anisole, 2-naphthylamines, 4-aminobphenyl, 4, 4 '-diaminodiphenyl ether, 4, 4 '-MDA, benzidine, 3, 3 '-dimethyl-4, 4 '-MDA, 3, 3 '-dimethylbenzidine, 4, 4 '-diaminodiphenyl sulfide, 3, 3 '-dichloro-benzidine, 3, 3 '-two chloro-4, 4 '-MDA, 3, 3 '-dimethylbenzidine, internal standard substance includes naphthalene-d8,245 trichloroaniline, anthracene-d10.
The mass spectrographic ion Selection parameter of described step (3) is in Table 3:
The quota ion of 321 kinds of aromatic amines of table and internal standard substance matter thereof and assisting ion
The present invention has the prominent advantages that: the step provided and method can be effectively used for measuring and move to specific aromatic amine migration amount in dry food analogies from paper and cardboard, and method is feasible, simple to operate, method is accurate, highly sensitive, the response rate is good, has application value.
Accompanying drawing explanation
Fig. 1 adopts gas chromatography/mass spectrometry method to analyze the total ions chromatogram of mixed standard solution in embodiment 1 step (4).
Wherein, 1) ortho-aminotoluene, 2) 2, 4-dimethylaniline, 3) 2, 6-dimethylaniline, 4) o-aminoanisole, 5) parachloroanilinum, 6) 2, 4, 5-trimethylaniline, 7) 2-methoxyl group-5-monomethylaniline., 8) 4-chloro-o-toluidine, 9) 2, 4-diaminotoluene, 10) 2, 4-diamino anisole, 11) 2-naphthylamines, 12) 4-aminobphenyl, 13) 4, 4-diaminodiphenyl ether, 14) 4, 4 '-MDA, 15) benzidine, 16) 3, 3 '-dimethyl-4, 4-MDA, 17) 3, 3 '-dimethylbenzidine, 18) 4, 4 '-diaminodiphenyl sulfide, 19) 3, 3 '-two chloro-4, 4 '-MDA, 20) 3, 3 '-dichloro-benzidine, 21) 3, 3 '-dimethylbenzidine, IS1) naphthalene-d8, IS2) 2, 4, 5-trichloroaniline, IS3) anthracene-d10.
Detailed description of the invention
The present invention is further described below with reference to embodiment, but is not limiting as the present invention.
Embodiments of the invention adopt following instrument and reagent:
Instrument: Clarus600 gas chromatograph (GC) (PerkinElmer, the U.S.);Clarus600T mass spectrograph (MS) (PerkinElmer, the U.S.);
Agents useful for same and material: t-butyl methyl ether, ethyl acetate (chromatographically pure, Merck, Germany); Tenax adsorbent, 60/80 order (CNWTechnologiesGmbH, Germany).
Embodiment 1
(1) art post paperboard to be measured is cut into 0.6dm2Sample, be taken as sample to be tested, sample to be tested be laid in container bottom, with Food Contact facing to upper, tile 3gTenax on sample to be tested surface, then be placed at 150 DEG C constant temperature and keep 24h, is cooled to room temperature; Time conditions and the temperature conditions of employing table 1 and table 2 are controlled:
The time conditions of table 1 test
| It is contemplated that the most sternly use when time of contact | Test period |
| t≤5 min | 5 min |
| 5 min≤t≤ 0.5 h | 0.5 h |
| 0.5 h≤t≤ 1 h | 1 h |
| 1 h≤t≤ 2 h | 2 h |
| 2 h≤t≤ 4 h | 4 h |
| 4 h≤t≤ 24 h | 24 h |
| T > 24 h | 240 h |
The temperature conditions of table 2 test
| It is contemplated that the most sternly use when Contact Temperature | Test temperature |
| T≤5 ℃ | 5 ℃ |
| 5 DEG C of < T≤20 DEG C | 20 ℃ 4 --> |
| 20 DEG C of < T≤40 DEG C | 40 ℃ |
| 40 DEG C of < T≤70 DEG C | 70 ℃ |
| 70 DEG C of < T≤100 DEG C | 100 DEG C or reflux temperature |
| 100 DEG C of < T≤121 DEG C | 121 ℃ |
| 121 DEG C of < T≤130 DEG C | 130 ℃ |
| 130 DEG C of < T≤150 DEG C | 150 ℃ |
| T > 150 DEG C | 175 ℃ |
(2) sample to be tested 3.0g in step (1) is taken out, it is placed in tool plug triangular flask and obtains extracting solution by solid-to-liquid ratio (g/mL) for the 1:10 ethyl acetate-t-butyl methyl ether solution at room temperature mechanical shaking extraction 0.5h adding 1:1 (v/v), again by extracting solution in 35 DEG C of nitrogen blow be concentrated into dry, add 2.0mL t-butyl methyl ether dissolve to obtain lysate;
(3) lysate in aspiration step (2), cross 0.22 μm of organic system microporous filter membrane, setting the selection ion of specific aromatic amine and internal standard substance by table 3, adopt gas chromatography/mass spectrometry method analysis to obtain the quota ion peak area of specific aromatic amine and internal standard substance in lysate, instrument condition is as follows:
The condition of gas chromatogram is chromatographic column DB-5 elastic capillary-column [fixing mutually for (50% phenyl)-methyl polysiloxane], 30m (length) × 0.25mm (internal diameter) × 0.25 μm (thickness); Injector temperature: 250 DEG C; Carrier gas: helium (purity >=99.999%); Constant current flow velocity: 1.0mL/min; Sample size: 1 μ L; Split ratio 10:1; Heating schedule: initial temperature 50 DEG C, keep 1min, with 5 DEG C/min to 280 DEG C, keep 8min;
Mass spectrographic condition is ion source: EI source; Ion source temperature: 230 DEG C; Ionizing energy: 70eV; Scan mode: full scan and selection ion scan (SIM); Sweep limits: m/z35～270amu; Solvent delay: 9.0min; Interface temperature: 280 DEG C; Mass spectrographic ion Selection parameter is in Table 3:
The quota ion of 321 kinds of aromatic amines of table and internal standard substance matter thereof and assisting ion
(4) the serial mixed standard solution of 21 kinds of aromatic amines is prepared with t-butyl methyl ether for solvent, series standard solution concentration is 0.5 μ g/mL, 2.5 μ g/mL, 5 μ g/mL, 10 μ g/mL, 25 μ g/mL, it is simultaneously introduced interior mark: naphthalene-d8,2,4,5-trichloroaniline, anthracene-d10, interior mark concentration is 2.5 μ g/mL; Series standard solution is carried out gas chromatograph-mass spectrometer (GC-MS) analysis, in each titer, the peak area of 21 kinds of aromatic amine quota ions and the quota ion peak area ratio at interior mark peak are for vertical coordinate, in each standard working solution, the content of 21 kinds of aromatic amines is for abscissa, makes the standard curve of 21 kinds of aromatic amines; The total ions chromatogram of 21 kinds of aromatic amine standard substances and internal standard substance is as shown in Figure 1.
(5) according to step (4) gained standard curve, in lysate, the quota ion peak area of each aromatic amine and internal standard substance substitutes into standard curve and calculates the concentration obtaining aromatic amine, and in sample to be tested, the migration amount of specific aromatic amine is calculated by formula (1):
... ... ... ... ... ... (1)
In formula:
The migration amount of specific aromatic amine in X sample, unit is microgram every square decimeter (μ g/dm2);
C is drawn the concentration of each aromatic amine in lysate by standard curve, and unit is micrograms per millilitre (μ g/mL); Being specially ortho-aminotoluene 0.62 μ g/mL, 2,4-dimethylaniline 0.52 μ g/mL, 4-aminobphenyl 0.65 μ g/mL, all the other all do not detect.
Redissolving the volume of solvent after the concentration of V extracting solution, unit is milliliter (mL), is specially 2mL;
The area of s sample to be tested, unit square decimetre (dm2), it is specially 0.6dm2;
It is 2.1 μ g/dm that calculating obtains ortho-aminotoluene migration amount2, 2,4-dimethylaniline migration amount is 1.7 μ g/dm2, 4-aminobphenyl migration amount is 2.2 μ g/dm2, do not detect other aromatic amines. According to the method described above, the relative standard deviation of 3 parallel determinations is 7.8～9.6%, illustrates that this method measures and migrates aromatic amine reliable results, and precision is good.
Embodiment 2
(1) template to be measured is cut into 1.0dm2Sample, be taken as sample to be tested, sample to be tested be laid in container bottom, with Food Contact facing to upper, tile 5gTenax on sample to be tested surface, then be placed at 20 DEG C constant temperature and keep 240h, is cooled to room temperature; Time conditions and the temperature conditions of employing table 1 and table 2 are controlled;
(2) Tenax5.0g of sample to be tested in step (1) is taken out, it is placed in tool plug triangular flask and obtains extracting solution by solid-to-liquid ratio (g/mL) for the 1:10 ethyl acetate-t-butyl methyl ether solution at room temperature mechanical shaking extraction 0.5h adding 1:1 (v/v), again by extracting solution in 35 DEG C of nitrogen blow be concentrated into dry, add 2.0mL t-butyl methyl ether dissolve to obtain lysate;
(3) with embodiment 1;
(4) with embodiment 1;
(5) according to step (4) gained standard curve, in lysate, the quota ion peak area of each aromatic amine and internal standard substance substitutes into standard curve and calculates the concentration obtaining aromatic amine, and in sample to be tested, the migration amount of specific aromatic amine is calculated by formula (1):
... ... ... ... ... ... (1)
In formula:
The migration amount of specific aromatic amine in X sample, unit is microgram every square decimeter (μ g/dm2);
The concentration of each aromatic amine in the lysate that C is drawn by standard curve, unit is micrograms per millilitre (μ g/mL); It is specially and does not all detect aromatic amine.
Redissolving the volume of solvent after the concentration of V extracting solution, unit is milliliter (mL), is specially 2mL;
The area of s sample to be tested, unit square decimetre (dm2), it is specially 1.0dm2;
This enforcement row do not detect the migration of aromatic amine.
Embodiment 3
(1) Paper or cardboard to be measured is cut into 0.2dm2Sample, be taken as sample to be tested, sample to be tested be laid in container bottom, with Food Contact facing to upper, tile 1gTenax on sample to be tested surface, then be placed at 100 DEG C constant temperature and keep 5min, is cooled to room temperature; Time conditions and the temperature conditions of employing table 1 and table 2 are controlled;
(2) Tenax1.0g of sample to be tested in step (1) is taken out, it is placed in tool plug triangular flask and obtains extracting solution by solid-to-liquid ratio (g/mL) for the 1:10 ethyl acetate-t-butyl methyl ether solution at room temperature mechanical shaking extraction 0.5h adding 1:1 (v/v), again by extracting solution in 35 DEG C of nitrogen blow be concentrated into dry, add 2.0mL t-butyl methyl ether dissolve to obtain lysate;
(3) with embodiment 1;
(4) with embodiment 1;
(5) according to step (4) gained standard curve, in lysate, the quota ion peak area of each aromatic amine and internal standard substance substitutes into standard curve and calculates the concentration obtaining aromatic amine, and in sample to be tested, the migration amount of specific aromatic amine is calculated by formula (1):
... ... ... ... ... ... (1)
In formula:
The migration amount of specific aromatic amine in X sample, unit is microgram every square decimeter (μ g/dm2);
C is drawn the concentration of each aromatic amine in lysate by standard curve, and unit is micrograms per millilitre (μ g/mL); Being specially ortho-aminotoluene 0.61 μ g/mL, all the other all do not detect.
Redissolving the volume of solvent after the concentration of V extracting solution, unit is milliliter (mL), is specially 2mL;
The area of s sample to be tested, unit square decimetre (dm2), it is specially 0.2dm2;
It is 6.1 μ g/dm that calculating obtains ortho-aminotoluene migration amount2, do not detect other aromatic amines.
Embodiment 4
(1) Paper or cardboard to be measured is cut into 0.4dm2Sample, be taken as sample to be tested, sample to be tested be laid in container bottom, with Food Contact facing to upper, tile 2gTenax on sample to be tested surface, then be placed at 5 DEG C constant temperature and keep 240h, is cooled to room temperature; Time conditions and the temperature part of employing table 1 and table 2 are controlled;
(2) Tenax2.0g of sample to be tested in step (1) is taken out, it is placed in tool plug triangular flask and obtains extracting solution by solid-to-liquid ratio (g/mL) for the 1:10 ethyl acetate-t-butyl methyl ether solution at room temperature mechanical shaking extraction 0.5h adding 1:1 (v/v), again by extracting solution in 35 DEG C of nitrogen blow be concentrated into dry, add 2.0mL t-butyl methyl ether dissolve to obtain lysate;
(3) with embodiment 1;
(4) with embodiment 1;
(5) according to step (4) gained standard curve, in lysate, the quota ion peak area of each aromatic amine and internal standard substance substitutes into standard curve and calculates the concentration obtaining aromatic amine, and in sample to be tested, the migration amount of specific aromatic amine is calculated by formula (1):
... ... ... ... ... ... (1)
In formula:
The migration amount of specific aromatic amine in X sample, unit is microgram every square decimeter (μ g/dm2);
C is drawn the concentration of each aromatic amine in lysate by standard curve, and unit is micrograms per millilitre (μ g/mL); It is specially and does not all detect aromatic amine.
Redissolving the volume of solvent after the concentration of V extracting solution, unit is milliliter (mL), is specially 2mL;
The area of s sample to be tested, unit square decimetre (dm2), it is specially 0.4dm2;
This enforcement row do not detect the migration of aromatic amine.
Claims (1)
1. one kind measures the method for aromatic amine migration amount in paper and cardboard, it is characterised in that through following each step:
(1) Paper or cardboard to be measured is cut into 0.2～1.0dm2Sample, be taken as sample to be tested, sample to be tested be laid in container bottom, with Food Contact facing to upper, the tiling amount of tile on sample to be tested surface Tenax, Tenax is by every dm2Sample to be tested add 5g, then be placed at 5～150 DEG C constant temperature and keep 5min～240h, be cooled to room temperature;
(2) Tenax1.0～5.0g of sample to be tested in step (1) is taken out, it is that 1:10 adds solvent and at room temperature carries out mechanical shaking extraction 0.5h and obtain extracting solution by solid-to-liquid ratio, solvent is the ethyl acetate-t-butyl methyl ether solution of 1:1v/v, again by extracting solution in 35 DEG C of nitrogen blow be concentrated into dry, add 2.0mL t-butyl methyl ether dissolve to obtain lysate;
(3) lysate of aspiration step (2), cross 0.22 μm of organic system microporous filter membrane, arranging the ion Selection parameter of specific aromatic amine and internal standard substance, adopt gas chromatography/mass spectrometry method analysis to obtain the quota ion peak area of each aromatic amine and internal standard substance in lysate, instrument condition is as follows:
The condition of gas chromatogram is chromatographic column DB-5 elastic capillary-column, and fixing is 50% PHENYL-METHYL polysiloxanes mutually, length 30m × internal diameter 0.25mm × thickness 0.25 μm;Injector temperature: 250 DEG C; Carrier gas: helium purity >=99.999%; Constant current flow velocity: 1.0mL/min; Sample size: 1 μ L; Split ratio 10:1; Heating schedule: initial temperature 50 DEG C, keeps 1min, rises to 280 DEG C with the speed of 5 DEG C/min, keeps 8min;
Mass spectrographic condition is ion source: EI source; Ion source temperature: 230 DEG C; Ionizing energy: 70eV; Scan mode: full scan and selection ion scan (SIM); Sweep limits: m/z35～270amu; Solvent delay: 9.0min; Interface temperature: 280 DEG C;
Described specific aromatic amine is ortho-aminotoluene, 2, 4-dimethylaniline, 2, 6-dimethylaniline, o-aminoanisole, parachloroanilinum, 2, 4, 5-trimethylaniline, 2-methoxyl group-5-monomethylaniline., 4-chloro-o-toluidine, 2, 4-diaminotoluene, 2, 4-diamino anisole, 2-naphthylamines, 4-aminobphenyl, 4, 4 '-diaminodiphenyl ether, 4, 4 '-MDA, benzidine, 3, 3 '-dimethyl-4, 4 '-MDA, 3, 3 '-dimethylbenzidine, 4, 4 '-diaminodiphenyl sulfide, 3, 3 '-dichloro-benzidine, 3, 3 '-two chloro-4, 4 '-MDA, 3, 3 '-dimethylbenzidine, internal standard substance includes naphthalene-d8,245 trichloroaniline, anthracene-d10,
(4) the serial mixed standard solution of above-mentioned 21 kinds of aromatic amines is prepared with t-butyl methyl ether for solvent, series standard solution concentration is 0.5 μ g/mL, 2.5 μ g/mL, 5 μ g/mL, 10 μ g/mL, 25 μ g/mL, it is simultaneously introduced interior mark: naphthalene-d8,2,4,5-trichloroaniline, anthracene-d10, interior mark concentration is 2.5 μ g/mL; Series standard solution is carried out gas chromatograph-mass spectrometer (GC-MS) analysis, in each titer, the peak area of 21 kinds of aromatic amine quota ions and the quota ion peak area ratio at interior mark peak are for vertical coordinate, in each standard working solution, the concentration of 21 kinds of aromatic amines is for abscissa, makes the standard curve of 21 kinds of aromatic amines;
(5) according to step (4) gained standard curve, the quota ion peak area of each aromatic amine and internal standard substance in lysate, substitute into standard curve and calculate the concentration obtaining aromatic amine, in sample to be tested, the migration amount of specific aromatic amine is calculated by formula (1):
... ... ... ... ... ... (1)
In formula:
The migration amount of specific aromatic amine in X sample, unit is microgram every square decimeter (μ g/dm2);
C is drawn the concentration of aromatic amine in lysate by standard curve, and unit is micrograms per millilitre (μ g/mL);
Redissolving the volume of solvent after the concentration of V extracting solution, unit is milliliter (mL),
The area of s sample to be tested, unit square decimetre (dm2).
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| CN110514752B (en) * | 2019-07-26 | 2022-03-11 | 云南中烟工业有限责任公司 | Extraction method of additive in paper food packaging material and non-targeted screening method thereof |
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| CN115201382A (en) * | 2022-09-08 | 2022-10-18 | 沧州大化股份有限公司 | Method for detecting sample containing diaminotoluene |
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Non-Patent Citations (6)
| Title |
|---|
| A study on the migration of organic pollutants from recycled paperboard packaging materials to solid food matrices;V.I.Triantafyllou等;《Food Chemistry》;20071231;第101卷;第1759～1768页 * |
| Migration of organic compounds from a multilayer plastic-paper material intended for food packaging;Cristina Nerin等;《Analytical and Bioanalytical Chemistry》;20070807;第389卷;第589～596页 * |
| Recycled paper-paperboard for food contact materials:contaminants suspected and migration into foods and food simulant;Nicoleta A.Suciu等;《Food Chemistry》;20130710;第141卷;第4146～4151页 * |
| 气相色谱-质谱法同时测定塑料食品接触材料中25种芳香族伯胺的迁移量;李英等;《色谱》;20130131;第31卷(第1期);第1.2.2节 * |
| 纸质食品包装材料中禁用芳香胺迁移量的测定;王成云等;《中国造纸》;20111231;第30卷(第11期);第7页左栏第1-2行，第1.2节，第1.3节，第1.4节，第2.7节，表1 * |
| 食品包装纸中模拟污染物迁移行为的研究;黄崇杏等;《食品科技》;20111231;第36卷(第6期);摘要，第1.4节 * |
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