CN104237438A - Method of utilizing Tenax as simulant with GCMS (Gas Chromatography Mass Spectrometry) to determine transfer volume of aromatic amine in paper and paperboard - Google Patents
Method of utilizing Tenax as simulant with GCMS (Gas Chromatography Mass Spectrometry) to determine transfer volume of aromatic amine in paper and paperboard Download PDFInfo
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Abstract
The invention discloses a method for determining a transfer volume of aromatic amine in paper and a paperboard. The method comprises the following steps: taking the modified polyphenyl ether as a simulant, conducting solvent extraction on the simulant, concentrating the extract liquor, and carrying out the GC/MS method to determine the transfer volume. The steps and the method provided by the invention can be effectively used for determining the transfer volume of the specific aromatic amine which is transferred from the paper and the paperboard to the dry food simulant; the method is feasible, simple to operate, accurate in method, high in sensitivity, and of value for popularization and application.
Description
Technical field
The present invention relates to a kind of method measuring specific aromatic amine migration amount in paper and paperboard, be specifically related to the polyphenylene oxide (MPPO adopting improvement, Tenax) as analogies, analogies, through solvent extraction, measure the aromatic amine of migration through GC-MS(gas chromatography-mass spectrography) (GC/MS) after extract is concentrated.
Background technology
Paper wrapper, as the important wrappage of a class, be widely used, and these wrapping papers is understood impressing pattern or word usually, likely uses the coating containing azo dyes.Part azo dyes can decompose under certain condition and discharges aromatic amine, and many aromatic amines are to health and bad environmental, and especially 2,4-xylidins, 2-naphthylamines, parachloroanilinum, biphenylamine, 4-aminobphenyl etc. are carcinogens.When paper wrapper is direct and Food Contact, the harmful aromatic amine wherein contained may move and enter into food, brings high risks to human health, therefore strictly must limit it from wrappage to the migration food.
Whether investigate harmful aromatic amine to move, whether the amount of migration reaches the level jeopardizing human health, direct investigation mode is exactly detect contained amount of moving aromatic amine in the food contacted with packaging Paper or cardboard.Owing to being difficult to carry out migration quantifier elimination to each food, namely most effective method is chosen suitable analogies and is set up migration models, obtains migration amount.But both at home and abroad relevant laws and regulations and document there is not yet migration models by setting up dry food analogies and method, carrying out aromatic amine in paper wrapper and moving to research in dry food.
Using Tenax as the analogies of dry food, in conjunction with gas chromatography/mass spectrometry method, the concrete operation step and the method that move to harmful aromatic amine in dry food analogies in foundation mensuration paper and paperboard are very meaningful.
Summary of the invention
For filling up the vacancy of prior art, the invention provides a kind of method measuring specific aromatic amine migration amount in paper and paperboard, be specifically related to the polyphenylene oxide (MPPO adopting improvement, Tenax) as analogies, analogies are through solvent extraction, and extract measures the aromatic amine of migration through GC-MS(gas chromatography-mass spectrography) (GC/MS).
The object of the invention is to be achieved through the following technical solutions: a kind of method measuring aromatic amine migration amount in paper and paperboard, is characterized in that through following each step:
(1) Paper or cardboard to be measured is cut into 0.2 ~ 1.0 dm
2sample, be taken as sample to be tested, sample to be tested is laid in container bottom, with Food Contact facing to upper, at sample to be tested surface tiling Tenax, then at being placed in 5 ~ 150 DEG C, constant temperature keeps 5 min ~ 240 h, then is cooled to room temperature;
(2) Tenax 1.0 ~ 5.0 g of sample to be tested in step (1) is taken out, be placed in tool plug triangular flask to carry out extracting to obtain extract for 1:10 adds solvent by solid-to-liquid ratio (g/mL), being blown in 35 DEG C of nitrogen by extract is concentrated into dry again, adds 2.0 mL t-butyl methyl ether and dissolves to obtain lysate;
(3) lysate of aspiration step (2), cross 0.22 μm of organic system miillpore filter, arrange the ion Selection parameter of specific aromatic amine and internal standard compound, adopt the analysis of gas chromatography/mass spectrometry method to obtain the quota ion peak area of each aromatic amine and internal standard compound in lysate, instrument condition is as follows:
The condition of gas chromatography is chromatographic column DB-5 elastic capillary-column [Stationary liquid is (50% phenyl)-methyl polysiloxane], 30 m (length) × 0.25 mm (internal diameter) × 0.25 μm (thickness); Injector temperature: 250 DEG C; Carrier gas: helium (purity >=99.999%); Constant current flow velocity: 1.0 mL/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 8 min;
Mass spectrographic condition is ion gun: EI source; Ion source temperature: 230 DEG C; Ionization energy: 70 eV; Scan mode: full scan and Selective ion mode scanning (SIM); Sweep limit: m/z 35 ~ 270 amu; Solvent delay: 9.0 min; Interface temperature: 280 DEG C;
(4) take t-butyl methyl ether as the serial mixed standard solution that 21 kinds of aromatic amines prepared by 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, add interior mark: naphthalene-d8,2 simultaneously, 4,5-trichloroaniline, anthracene-d10, interior mark concentration is 2.5 μ g/mL
;gas chromatograph-mass spectrometer (GCMS) analysis is carried out to series standard solution, with the quota ion peak area ratio at the peak area of 21 kinds of aromatic amine quota ions in each titer and interior mark peak for ordinate, with the concentration of 21 kinds of aromatic amines in each standard working solution for horizontal ordinate, make the typical curve of 21 kinds of aromatic amines;
(5) according to step (4) gained typical curve, the quota ion peak area of each aromatic amine and internal standard compound in lysate, substitute into the concentration that typical curve calculates aromatic amine, in sample to be tested, the migration amount of specific aromatic amine calculates by formula (1):
?……………………?………（1）
In formula:
x---the migration amount of specific aromatic amine in sample, unit is microgram every square decimeter (μ g/dm
2);
c---drawn the concentration of aromatic amine in lysate by typical curve, unit is micrograms per millilitre (μ g/mL);
v---extract concentrates the volume of rear redissolution solvent, and unit is milliliter (mL).
In described step (1), the tiling amount of Tenax is by every dm
2sample to be tested add 5 g.
Being placed in constant temperature at 5 ~ 100 DEG C in described step (1) keeps the time conditions of 5 min ~ 240 h employing tables 1 and table 2 and temperature conditions to control:
The time conditions that table 1 is tested
| The duration of contact under the severeest service condition can be predicted | 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 that table 2 is tested
| The Contact Temperature under the severeest service condition can be predicted | Test temperature |
| T≤5 ℃ | 5 ℃ |
| 5 ℃＜ T≤20 ℃ | 20 ℃ |
| 20 ℃＜ T≤40 ℃ | 40 ℃ |
| 40 ℃＜ T≤70 ℃ | 70 ℃ |
| 70 ℃＜T≤100 ℃ | 100 DEG C or reflux temperature |
| 100 ℃＜ T≤121 ℃ | 121 ℃ |
| 121 ℃＜ T≤130 ℃ | 130 ℃ |
| 130 ℃＜ T≤150 ℃ | 150 ℃ |
| T＞150 ℃ | 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 0.5 h.
The specific aromatic amine of described step (3) comprises ortho-aminotoluene, 2, 4-xylidin, 2, 6-xylidin, o-aminoanisole, parachloroanilinum, 2, 4, 5-trimethylaniline, 2-methoxyl-5-methylaniline, 4-chloro-o-toluidine, 2, 4-diaminotoluene, 2, 4-diamino anisole, 2-naphthylamines, 4-aminobphenyl, 4, 4 '-diaminodiphenyl ether, 4, 4 '-diaminodiphenylmethane, biphenylamine, 3, 3 '-dimethyl-4, 4 '-diaminodiphenylmethane, 3, 3 '-dimethylbenzidine, 4, 4 '-diaminodiphenyl sulfide, 3, 3 '-dichloro-benzidine, 3, 3 '-two chloro-4, 4 '-diaminodiphenylmethane, 3, 3 '-dimethylbenzidine, internal standard compound comprises naphthalene-d8,2,4,5-trichloroanilines, anthracene-d10.
The mass spectrographic ion Selection parameter of described step (3) is in table 3:
The quota ion of table 3 21 kinds of aromatic amines and internal standard compound matter thereof and assisting ion
Outstanding advantages of the present invention is: the step and method provided can be effective to measure from paper and paperboard, move to specific aromatic amine migration amount in dry food analogies, and method is feasible, simple to operate, method is accurate, highly sensitive, the recovery 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-xylidin, 3) 2, 6-xylidin, 4) o-aminoanisole, 5) parachloroanilinum, 6) 2, 4, 5-trimethylaniline, 7) 2-methoxyl-5-methylaniline, 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 '-diaminodiphenylmethane, 15) biphenylamine, 16) 3, 3 '-dimethyl-4, 4-diaminodiphenylmethane, 17) 3, 3 '-dimethylbenzidine, 18) 4, 4 '-diaminodiphenyl sulfide, 19) 3, 3 '-two chloro-4, 4 '-diaminodiphenylmethane, 20) 3, 3 '-dichloro-benzidine, 21) 3, 3 '-dimethylbenzidine, IS1) naphthalene-d8, IS2) 2, 4, 5-trichloroaniline, IS3) anthracene-d10.
Embodiment
The present invention is further described below with reference to embodiment, but does not limit the present invention.
Embodiments of the invention adopt following instrument and reagent:
Instrument: Clarus 600 gas chromatograph (GC) (PerkinElmer, the U.S.); Clarus 600T mass spectrometer (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 (CNW Technologies GmbH, Germany).
Embodiment 1
(1) art post paperboard to be measured is cut into 0.6 dm
2sample, be taken as sample to be tested, sample to be tested is laid in container bottom, with Food Contact facing to upper, at sample to be tested surface tiling 3 g Tenax, then at being placed in 150 DEG C, constant temperature keeps 24 h, then is cooled to room temperature; Time conditions and the temperature conditions of employing table 1 and table 2 control:
The time conditions that table 1 is tested
| The duration of contact under the severeest service condition can be predicted | 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 that table 2 is tested
| The Contact Temperature under the severeest service condition can be predicted | Test temperature |
| T≤5 ℃ | 5 ℃ |
| 5 ℃＜ T≤20 ℃ | 20 ℃ |
| 20 ℃＜ T≤40 ℃ | 40 ℃ |
| 40 ℃＜ T≤70 ℃ | 70 ℃ |
| 70 ℃＜T≤100 ℃ | 100 DEG C or reflux temperature |
| 100 ℃＜ T≤121 ℃ | 121 ℃ |
| 121 ℃＜ T≤130 ℃ | 130 ℃ |
| 130 ℃＜ T≤150 ℃ | 150 ℃ |
| T＞150 ℃ | 175 ℃ |
(2) sample to be tested 3.0 g in step (1) is taken out, be placed in ethyl acetate-t-butyl methyl ether solution that tool plug triangular flask adds 1:1 (v/v) by solid-to-liquid ratio (g/mL) for 1:10 at room temperature mechanical shaking extraction 0.5 h obtain extract, being blown in 35 DEG C of nitrogen by extract is concentrated into dry again, adds 2.0 mL t-butyl methyl ether and dissolves to obtain lysate;
(3) lysate in aspiration step (2), cross 0.22 μm of organic system miillpore filter, set the Selective ion mode of specific aromatic amine and internal standard compound by table 3, adopt the analysis of gas chromatography/mass spectrometry method to obtain the quota ion peak area of specific aromatic amine and internal standard compound in lysate, instrument condition is as follows:
The condition of gas chromatography is chromatographic column DB-5 elastic capillary-column [Stationary liquid is (50% phenyl)-methyl polysiloxane], 30 m (length) × 0.25 mm (internal diameter) × 0.25 μm (thickness); Injector temperature: 250 DEG C; Carrier gas: helium (purity >=99.999%); Constant current flow velocity: 1.0 mL/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 8 min;
Mass spectrographic condition is ion gun: EI source; Ion source temperature: 230 DEG C; Ionization energy: 70 eV; Scan mode: full scan and Selective ion mode scanning (SIM); Sweep limit: m/z 35 ~ 270 amu; Solvent delay: 9.0 min; Interface temperature: 280 DEG C; Mass spectrographic ion Selection parameter is in table 3:
The quota ion of table 3 21 kinds of aromatic amines and internal standard compound matter thereof and assisting ion
(4) take t-butyl methyl ether as the serial mixed standard solution that 21 kinds of aromatic amines prepared by 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, add interior mark: naphthalene-d8,2 simultaneously, 4,5-trichloroaniline, anthracene-d10, interior mark concentration is 2.5 μ g/mL
;gas chromatograph-mass spectrometer (GCMS) analysis is carried out to series standard solution, with the quota ion peak area ratio at the peak area of 21 kinds of aromatic amine quota ions in each titer and interior mark peak for ordinate, with the content of 21 kinds of aromatic amines in each standard working solution for horizontal ordinate, make the typical curve of 21 kinds of aromatic amines; The total ions chromatogram of 21 kinds of aromatic amine standard substances and internal standard compound as shown in Figure 1.
(5) according to step (4) gained typical curve, in lysate, the quota ion peak area of each aromatic amine and internal standard compound substitutes into the concentration that typical curve calculates aromatic amine, and in sample to be tested, the migration amount of specific aromatic amine calculates by formula (1):
?……………………?………（1）
In formula:
x---the migration amount of specific aromatic amine in sample, unit is microgram every square decimeter (μ g/dm
2);
c---drawn the concentration of each aromatic amine in lysate by typical curve, unit is micrograms per millilitre (μ g/mL); Be specially ortho-aminotoluene 0.62 μ g/mL, 2,4-xylidin 0.52 μ g/mL, 4-aminobphenyl 0.65 μ g/mL, all the other all do not detect.
v---extract concentrates the volume of rear redissolution solvent, and unit is milliliter (mL), is specially 2 mL;
s---the area of sample to be tested, unit square decimetre (dm
2), be specially 0.6 dm
2;
Calculating ortho-aminotoluene migration amount is 2.1 μ g/dm
2, 2,4-xylidin migration amount is 1.7 μ g/ dm
2, 4-aminobphenyl migration amount is 2.2 μ g/dm
2, 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%, and illustrate that this method measures migration aromatic amine reliable results, precision is good.
Embodiment 2
(1) template to be measured is cut into 1.0 dm
2sample, be taken as sample to be tested, sample to be tested is laid in container bottom, with Food Contact facing to upper, at sample to be tested surface tiling 5 g Tenax, then at being placed in 20 DEG C, constant temperature keeps 240 h, then is cooled to room temperature; Time conditions and the temperature conditions of employing table 1 and table 2 control;
(2) Tenax 5.0 g of sample to be tested in step (1) is taken out, be placed in ethyl acetate-t-butyl methyl ether solution that tool plug triangular flask adds 1:1 (v/v) by solid-to-liquid ratio (g/mL) for 1:10 at room temperature mechanical shaking extraction 0.5 h obtain extract, being blown in 35 DEG C of nitrogen by extract is concentrated into dry again, adds 2.0 mL t-butyl methyl ether and dissolves to obtain lysate;
(3) with embodiment 1;
(4) with embodiment 1;
(5) according to step (4) gained typical curve, in lysate, the quota ion peak area of each aromatic amine and internal standard compound substitutes into the concentration that typical curve calculates aromatic amine, and in sample to be tested, the migration amount of specific aromatic amine calculates by formula (1):
?……………………?………（1）
In formula:
x---the migration amount of specific aromatic amine in sample, unit is microgram every square decimeter (μ g/dm
2);
c---the concentration of each aromatic amine in the lysate drawn by typical curve, unit is micrograms per millilitre (μ g/mL); Be specially and all do not detect aromatic amine.
v---extract concentrates the volume of rear redissolution solvent, and unit is milliliter (mL), is specially 2 mL;
s---the area of sample to be tested, unit square decimetre (dm
2), be specially 1.0 dm
2;
The migration of aromatic amine is not detected in this implementation column.
Embodiment 3
(1) Paper or cardboard to be measured is cut into 0.2 dm
2sample, be taken as sample to be tested, sample to be tested is laid in container bottom, with Food Contact facing to upper, at sample to be tested surface tiling 1 g Tenax, then at being placed in 100 DEG C, constant temperature keeps 5 min, then is cooled to room temperature; Time conditions and the temperature conditions of employing table 1 and table 2 control;
(2) Tenax 1.0 g of sample to be tested in step (1) is taken out, be placed in ethyl acetate-t-butyl methyl ether solution that tool plug triangular flask adds 1:1 (v/v) by solid-to-liquid ratio (g/mL) for 1:10 at room temperature mechanical shaking extraction 0.5 h obtain extract, being blown in 35 DEG C of nitrogen by extract is concentrated into dry again, adds 2.0 mL t-butyl methyl ether and dissolves to obtain lysate;
(3) with embodiment 1;
(4) with embodiment 1;
(5) according to step (4) gained typical curve, in lysate, the quota ion peak area of each aromatic amine and internal standard compound substitutes into the concentration that typical curve calculates aromatic amine, and in sample to be tested, the migration amount of specific aromatic amine calculates by formula (1):
?……………………?………（1）
In formula:
x---the migration amount of specific aromatic amine in sample, unit is microgram every square decimeter (μ g/dm
2);
c---drawn the concentration of each aromatic amine in lysate by typical curve, unit is micrograms per millilitre (μ g/mL); Be specially ortho-aminotoluene 0.61 μ g/mL, all the other all do not detect.
v---extract concentrates the volume of rear redissolution solvent, and unit is milliliter (mL), is specially 2 mL;
s---the area of sample to be tested, unit square decimetre (dm
2), be specially 0.2 dm
2;
Calculating ortho-aminotoluene migration amount is 6.1 μ g/dm
2, do not detect other aromatic amines.
Embodiment 4
(1) Paper or cardboard to be measured is cut into 0.4 dm
2sample, be taken as sample to be tested, sample to be tested is laid in container bottom, with Food Contact facing to upper, at sample to be tested surface tiling 2 g Tenax, then at being placed in 5 DEG C, constant temperature keeps 240 h, then is cooled to room temperature; Time conditions and the temperature part of employing table 1 and table 2 control;
(2) Tenax 2.0 g of sample to be tested in step (1) is taken out, be placed in ethyl acetate-t-butyl methyl ether solution that tool plug triangular flask adds 1:1 (v/v) by solid-to-liquid ratio (g/mL) for 1:10 at room temperature mechanical shaking extraction 0.5 h obtain extract, being blown in 35 DEG C of nitrogen by extract is concentrated into dry again, adds 2.0 mL t-butyl methyl ether and dissolves to obtain lysate;
(3) with embodiment 1;
(4) with embodiment 1;
(5) according to step (4) gained typical curve, in lysate, the quota ion peak area of each aromatic amine and internal standard compound substitutes into the concentration that typical curve calculates aromatic amine, and in sample to be tested, the migration amount of specific aromatic amine calculates by formula (1):
?……………………?………（1）
In formula:
x---the migration amount of specific aromatic amine in sample, unit is microgram every square decimeter (μ g/dm
2);
c---drawn the concentration of each aromatic amine in lysate by typical curve, unit is micrograms per millilitre (μ g/mL); Be specially and all do not detect aromatic amine.
v---extract concentrates the volume of rear redissolution solvent, and unit is milliliter (mL), is specially 2 mL;
s---the area of sample to be tested, unit square decimetre (dm
2), be specially 0.4 dm
2;
The migration of aromatic amine is not detected in this implementation column.
Claims (5)
1. measure a method for aromatic amine migration amount in paper and paperboard, it is characterized in that through following each step:
(1) Paper or cardboard to be measured is cut into 0.2 ~ 1.0 dm
2sample, be taken as sample to be tested, sample to be tested is laid in container bottom, with Food Contact facing to upper, at sample to be tested surface tiling Tenax, then at being placed in 5 ~ 150 DEG C, constant temperature keeps 5 min ~ 240 h, then is cooled to room temperature;
(2) taking out Tenax 1.0 ~ 5.0 g of sample to be tested in step (1), is that 1:10 adds solvent and carries out extracting to obtain extract by solid-to-liquid ratio, then is blown in 35 DEG C of nitrogen by extract and be concentrated into dry, adds 2.0 mL t-butyl methyl ether and dissolves to obtain lysate;
(3) lysate of aspiration step (2), cross 0.22 μm of organic system miillpore filter, arrange the ion Selection parameter of specific aromatic amine and internal standard compound, adopt the analysis of gas chromatography/mass spectrometry method to obtain the quota ion peak area of each aromatic amine and internal standard compound in lysate, instrument condition is as follows:
The condition of gas chromatography is chromatographic column DB-5 elastic capillary-column [Stationary liquid is (50% phenyl)-methyl polysiloxane], 30 m (length) × 0.25 mm (internal diameter) × 0.25 μm (thickness); Injector temperature: 250 DEG C; Carrier gas: helium (purity >=99.999%); Constant current flow velocity: 1.0 mL/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 8 min;
Mass spectrographic condition is ion gun: EI source; Ion source temperature: 230 DEG C; Ionization energy: 70 eV; Scan mode: full scan and Selective ion mode scanning (SIM); Sweep limit: m/z 35 ~ 270 amu; Solvent delay: 9.0 min; Interface temperature: 280 DEG C;
(4) take t-butyl methyl ether as the serial mixed standard solution that 21 kinds of aromatic amines prepared by 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, add interior mark: naphthalene-d8,2 simultaneously, 4,5-trichloroaniline, anthracene-d10, interior mark concentration is 2.5 μ g/mL
;gas chromatograph-mass spectrometer (GCMS) analysis is carried out to series standard solution, with the quota ion peak area ratio at the peak area of 21 kinds of aromatic amine quota ions in each titer and interior mark peak for ordinate, with the concentration of 21 kinds of aromatic amines in each standard working solution for horizontal ordinate, make the typical curve of 21 kinds of aromatic amines;
(5) according to step (4) gained typical curve, the quota ion peak area of each aromatic amine and internal standard compound in lysate, substitute into the concentration that typical curve calculates aromatic amine, in sample to be tested, the migration amount of specific aromatic amine calculates by formula (1):
?……………………?………（1）
In formula:
x---the migration amount of specific aromatic amine in sample, unit is microgram every square decimeter (μ g/dm
2);
c---drawn the concentration of aromatic amine in lysate by typical curve, unit is micrograms per millilitre (μ g/mL);
v---extract concentrates the volume of rear redissolution solvent, and unit is milliliter (mL).
2. the method for aromatic amine migration amount in mensuration paper and paperboard according to claim 1, is characterized in that: in described step (1), the tiling amount of Tenax is by every dm
2sample to be tested add 5 g.
3. the method for aromatic amine migration amount in mensuration paper and paperboard according to claim 1, is characterized in that: in described step (2), solvent is the ethyl acetate-t-butyl methyl ether solution of 1:1 (v/v).
4. the method for aromatic amine migration amount in mensuration paper and paperboard according to claim 1, is characterized in that: extracting in described step (2) is at room temperature mechanical shaking extraction 0.5 h.
5. the method for aromatic amine migration amount in mensuration paper and paperboard according to claim 1, it is characterized in that: the specific aromatic amine of described step (3) comprises ortho-aminotoluene, 2, 4-xylidin, 2, 6-xylidin, o-aminoanisole, parachloroanilinum, 2, 4, 5-trimethylaniline, 2-methoxyl-5-methylaniline, 4-chloro-o-toluidine, 2, 4-diaminotoluene, 2, 4-diamino anisole, 2-naphthylamines, 4-aminobphenyl, 4, 4 '-diaminodiphenyl ether, 4, 4 '-diaminodiphenylmethane, biphenylamine, 3, 3 '-dimethyl-4, 4 '-diaminodiphenylmethane, 3, 3 '-dimethylbenzidine, 4, 4 '-diaminodiphenyl sulfide, 3, 3 '-dichloro-benzidine, 3, 3 '-two chloro-4, 4 '-diaminodiphenylmethane, 3, 3 '-dimethylbenzidine, internal standard compound comprises naphthalene-d8,2,4,5-trichloroanilines, anthracene-d10.
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| CN107894480A (en) * | 2017-12-20 | 2018-04-10 | 上海建科检验有限公司 | A kind of GC-MS detection method of MOCA contents and its application |
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| CN113504333A (en) * | 2021-08-20 | 2021-10-15 | 上海烟草集团有限责任公司 | Method for detecting organic matter migration amount in paper packaging material |
| CN115201382A (en) * | 2022-09-08 | 2022-10-18 | 沧州大化股份有限公司 | Method for detecting sample containing diaminotoluene |
| CN117030919A (en) * | 2023-10-09 | 2023-11-10 | 山东欧亚高分子材料有限公司 | Gas chromatography detection method for 4,4' -diaminodiphenyl ether content |
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| CN110514752A (en) * | 2019-07-26 | 2019-11-29 | 云南中烟工业有限责任公司 | The extracting method of additive and its non-targeted screening method in a kind of paper food packaging materials |
| CN113504333A (en) * | 2021-08-20 | 2021-10-15 | 上海烟草集团有限责任公司 | Method for detecting organic matter migration amount in paper packaging material |
| CN113504333B (en) * | 2021-08-20 | 2023-03-14 | 上海烟草集团有限责任公司 | Method for detecting organic matter migration amount in paper packaging material |
| CN115201382A (en) * | 2022-09-08 | 2022-10-18 | 沧州大化股份有限公司 | Method for detecting sample containing diaminotoluene |
| CN117030919A (en) * | 2023-10-09 | 2023-11-10 | 山东欧亚高分子材料有限公司 | Gas chromatography detection method for 4,4' -diaminodiphenyl ether content |
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