CN102879510B - Method for detecting migration quantity of nipagin ester substances in plastic food package bag - Google Patents
Method for detecting migration quantity of nipagin ester substances in plastic food package bag Download PDFInfo
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Abstract
The invention provides a method for detecting the migration quantity of nipagin ester substances in a plastic food package bag. The method comprises the following steps of: making the plastic bag of the size of 10*10 cm<2> by a plastic sample to be detected through a plastic sealing machine, washing the plastic bag by using distilled water, and drying; respectively putting water-based food simulation liquid and olive oil into the plastic bags, and sealing to obtain a water-based food simulation liquid immersed solution and an olive oil immersed solution; performing simple treatment on the obtained immersed solutions to obtain solutions to be detected; performing analysis detection on the solutions to be detected by adopting high performance liquid chromatography (HPLC)/mass spectrum (MS)/mass spectrum (MS) to obtain theoretical measured values of the nipagin ester substances in the samples to be detected; and deducing blank values from the theoretical measured values to obtain actual measured values of the nipagin ester substances in the immersed solutions of the samples to be detected. By the method, the technical blank of detection for the nipagin ester substances in the plastic food package bag in China is filled; and the method has the characteristics of simplicity in operation and high detection accuracy.
Description
[technical field]
The present invention relates to a kind of detection method, relate in particular to the detection method of parabens material migration amount in a kind of plastic packing bag.
[background technology]
P-hydroxybenzoate, claims again nipagin esters, is that a class is safe, efficient, the antiseptic of wide spectrum, is widely used in the numerous areas such as food, beverage, cosmetics, medicine.Parabens antiseptic has phenolic hydroxyl structure, and antibacterium performance is all stronger than benzoic acid, sorbic acid, and all has very strong fungistatic effect at wider pH range 3-8.There is report to show, nipagin esters can be used as antiseptic and joins and in packaging material for food, prepare active food packaging, and the active component in active packing, by slowly discharging, changes the interior environmental conditions of packaging for foodstuff, extend the shelf life of food, improve the organoleptic quality of food.Thereby active food packaging technology becomes countries in the world, the technology emphasis that particularly developed country is studied.At present, the parabens antiseptic generally adopting in the world mainly contains methyl hydroxybenzoate, ethyl ester, propyl ester, isopropyl ester, butyl ester, isobutyl ester, heptyl ester and monooctyl ester.Wherein China is mainly used methyl hydroxybenzoate, ethyl ester and propyl ester, the main butyl hydroxybenzoate that uses of Japan, and the U.S. is mainly used heptyl paraben.
Although nipagin esters toxicity is lower, a large amount of uses still can be detrimental to health, and research shows that this type of antiseptic can cause optimum and malignant breast tumour, scytitis, disturbs the normal secretion of human endocrine hormone etc.Therefore the migration research of, carrying out parabens material has important practical significance.Via ISO, ASTM, GB, the standards such as SN are looked into and are newly had no relevant criterion report, through patent network inquiry, also have no Patents report.Therefore be badly in need of exploitation easy, the quantitative determination of parabens material migration fast detection method.
[summary of the invention]
Technical matters to be solved by this invention is to provide the detection method of parabens material migration amount in a kind of plastic packing bag, not only filled up the technological gap in the detection of China's parabens material in plastic packing bag, and have advantages of easy operating and detection accuracy high.
The present invention is the detection method of parabens material migration amount in a kind of plastic packing bag solving the problems of the technologies described above by the following technical programs, and it specifically comprises following operation steps:
Step 1, sample preparation: choose plastic sample and with plastic sealing machine, be made into the polybag of 10cm * 10cm, with distilled water, clean, dry; Get this polybag after drying and pack the water base food simulated solution of 200mL into, then get this polybag after drying and pack 200g olive oil into, then with capper sealing to obtain respectively water base food analogies soak solution and olive oil soak solution;
Step 2, sample purification:
(1) oil base food analogies: get the olive oil soak solution 0.5g that step 1 obtains, and add 3mL isooctane to dissolve, vortex 2min mixes to obtain mixed liquor, then mixed liquor is passed through to C
18post, with 6mL isooctane drip washing pillar and discard efflux, use again 9mL eluent ethyl acetate, collect eluent ethyl acetate liquid and be placed in nitrogen bottle blowing, then at 45 ℃, with nitrogen, liquid in nitrogen bottle blowing is dried up to obtain to residue, this residue is dissolved and the centrifugal 2min of 2500r/min with 1mL methyl alcohol, after centrifugal end, get supernatant and cross 0.22 μ m miillpore filter and obtain filtrate, obtain the liquid to be measured of oil base food analogies;
(2) water base food analogies: the water base food analogies soak solution 1mL that draws step 1 acquisition crosses 0.22 μ m miillpore filter and obtains filtrate, obtains the liquid to be measured of water base food analogies;
Step 3, analyzing and testing: all adopt HPLC/MS/MS to carry out analyzing and testing each liquid to be measured obtaining, particularly, it is the response signal of parabens material to obtain measured object in liquid to be measured that liquid to be measured is carried out to upper machine analysis, according to the response signal of measured object in liquid to be measured, choose the corresponding standard operation liquid of response afterwards and carry out stratographic analysis, standard operation liquid is provided with and comprises zero point in six interior concentration gradients, and in standard operation liquid and liquid to be measured, the response of parabens material all should be in instrument linear response range, and a blank is set simultaneously;
Step 4, testing result are calculated: HPLC/MS/MS is obtained to each parameter value substitution following formula (1) or formula (2) is calculated, to obtain the practical measurement value of parabens material in each liquid to be measured;
The migration amount of parabens material in the liquid to be measured of water base food analogies, by following formula (1), calculate:
In formula (1):
The migration amount of parabens material in X-liquid to be measured, unit is mg/kg;
The peak area of parabens material in A-liquid to be measured;
A
0the peak area of parabens material in-blank;
The peak area of parabens material in As-standard operation liquid;
The concentration of parabens material in c-standard operation liquid, unit is mg/L;
V-soak solution volume, unit is L;
The contact area of S-sample and oil base food analogies, unit is dm
2;
In 6-european union directive 2002/72/EC, stipulate mg/kg=6mg/dm
2;
The migration amount of nipagin esters in the liquid to be measured of oil base food analogies, by formula (2), calculate:
In formula (2):
The migration amount of parabens material in X-liquid to be measured, unit is mg/kg;
The peak area of parabens material in A-liquid to be measured;
A
0the peak area of parabens material in-blank;
The peak area of parabens material in As-standard operation liquid;
The concentration of parabens material in c-standard operation liquid, unit is mg/L;
During m-purification, take the quality of olive oil soak solution, unit is kg;
Constant volume after V-olive oil sample purification, unit is L;
In step 3, the HPLC condition in described HPLC/MS/MS is:
A chromatographic column: ZORBAX SB-C
18, 4.6mm * 150mm, granularity 5 μ m;
B mobile phase: methyl alcohol, water;
C gradient:
D sample size: 5 μ L;
E column temperature: 35 ℃;
And the MS/MS condition in described HPLC/MS/MS is:
A ' ion gun: Negative electrospray ionization source, multiple-reaction monitoring scan mode;
B ' capillary voltage: 4kV;
C ' ion source temperature: 350 ℃;
D ' atomizer pressure: 40psi;
E ' dry gas flow velocity: 8L/min;
The mass spectrum parameter optimization of 8 kinds of nipagin esters of f ':
And being wherein with ★ is quota ion.
Further, described water base food simulated solution is distilled water, 3% acetic acid or 10% ethanol.
In plastic packing bag of the present invention, the beneficial effect of the detection method of parabens material migration amount is: filled up the technological gap in the detection of China's parabens material in plastic packing bag, and have advantages of easy operating and detection accuracy high.
[embodiment]
The detection method of parabens material migration amount in plastic packing bag of the present invention, it specifically comprises following operation steps:
Step 1, sample preparation: choose plastic sample and with plastic sealing machine, be made into the polybag of 10cm * 10cm, with distilled water, clean, dry; Get this polybag after drying and pack the water base food simulated solution of 200mL (distilled water, 3% acetic acid or 10% ethanol) into, according to every 1cm
2ratio (the 2mL/cm of the water base food simulated solution of contact area contact 2mL
2); Get again this polybag after drying and pack 200g olive oil into, according to every 1cm
2ratio (the 2g/cm of contact area contact 2g oil base food simulated solution
2); Then with capper, seal to obtain respectively water base food analogies soak solution and olive oil soak solution;
Step 2, sample purification:
(1) oil base food analogies: get the olive oil soak solution 0.5g that step 1 obtains, and add 3mL isooctane to dissolve, vortex 2min mixes to obtain mixed liquor, then mixed liquor is passed through to C
18post, with 6mL isooctane drip washing pillar and discard efflux, use again 9mL eluent ethyl acetate, collect eluent ethyl acetate liquid and be placed in nitrogen bottle blowing, then at 45 ℃, with nitrogen, liquid in nitrogen bottle blowing is dried up to obtain to residue, this residue is dissolved and the centrifugal 2min of 2500r/min with 1mL methyl alcohol, after centrifugal end, get supernatant and cross 0.22 μ m miillpore filter and obtain filtrate, obtain the liquid to be measured of oil base food analogies;
(2) water base food analogies: the water base food analogies soak solution 1mL that draws step 1 acquisition crosses 0.22 μ m miillpore filter and obtains filtrate, obtains the liquid to be measured of water base food analogies;
Step 3, analyzing and testing: all adopt using high performance liquid chromatography tandem mass spectrum method (HPLC/MS/MS) to carry out analyzing and testing each liquid to be measured obtaining, particularly, it is the response signal of parabens material to obtain measured object in liquid to be measured that liquid to be measured is carried out to upper machine analysis, according to the response signal of measured object in liquid to be measured, choose the corresponding standard operation liquid of response afterwards and carry out stratographic analysis, standard operation liquid is provided with and comprises zero point in six interior concentration gradients, and in standard operation liquid and liquid to be measured, the response of parabens material all should be in instrument linear response range, and a blank is set simultaneously,
Step 4, testing result are calculated: HPLC/MS/MS is obtained to each parameter value substitution following formula (1) or formula (2) is calculated, to obtain the practical measurement value of parabens material in each liquid to be measured;
The migration amount of parabens material in the liquid to be measured of water base food analogies, by following formula (1), calculate:
In formula (1):
The migration amount of parabens material in X-liquid to be measured, unit is mg/kg;
The peak area of parabens material in A-liquid to be measured;
A
0the peak area of parabens material in-blank;
The peak area of parabens material in As-standard operation liquid;
The concentration of parabens material in c-standard operation liquid, unit is mg/L;
V-soak solution volume, unit is L;
The contact area of S-sample and oil base food analogies, unit is dm
2;
In 6-european union directive 2002/72/EC, stipulate mg/kg=6mg/dm
2;
The migration amount of nipagin esters in the liquid to be measured of oil base food analogies, by formula (2), calculate:
In formula (2):
The migration amount of parabens material in X-liquid to be measured, unit is mg/kg;
The peak area of parabens material in A-liquid to be measured;
A
0the peak area of parabens material in-blank;
The peak area of parabens material in As-standard operation liquid;
The concentration of parabens material in c-standard operation liquid, unit is mg/L;
During m-purification, take the quality of olive oil soak solution, unit is kg;
Constant volume after V-olive oil sample purification, unit is L;
Wherein, the HPLC condition in HPLC/MS/MS is:
A chromatographic column: ZORBAX SB-C
18, 4.6mm * 150mm, granularity 5 μ m;
B mobile phase: methyl alcohol, water;
C gradient:
D sample size: 5 μ L;
E column temperature: 35 ℃;
And the MS/MS condition in described HPLC/MS/MS is:
A ' ion gun: Negative electrospray ionization source, multiple-reaction monitoring scan mode;
B ' capillary voltage: 4kV;
C ' ion source temperature: 350 ℃;
D ' atomizer pressure: 40psi;
E ' dry gas flow velocity: 8L/min;
The mass spectrum parameter optimization of 8 kinds of nipagin esters of f ':
And being wherein with ★ is quota ion.
In addition, the mensuration lower bound of the inventive method is: a) water base food analogies are 2 μ g/kg; B) oil base food analogies are 4 μ g/kg.And four kinds of food analogies (be distilled water, 3% acetic acid, 10% ethanol, be olive oil) are good in 5~300 μ g/L scope internal standard curve linear relations, and correlation coefficient r is greater than 0.99.
In order better the present invention to be set forth to explanation, the application is for following several embodiment, and all the feasibility of detection method of the present invention and accuracy verified in each embodiment.
Embodiment mono-: testing sample---negative plastic packing bag (negative sample)
1.1 sample preparations: choose negative plastic food packing material (not containing the plastic food packing material of parabens material) and be made into the polybag of 10cm * 10cm with plastic sealing machine, clean with distilled water, dry; Get four these polybags after drying, and be labeled as respectively polybag I, polybag II, polybag III, polybag IV, in polybag I, polybag II, polybag III, be respectively charged into 200mL distilled water, 200mL3% acetic acid, 200mL10% ethanol, and in polybag IV, pack 200g olive oil into; Then with capper, seal each polybag to obtain respectively each water base food analogies soak solution and olive oil soak solution;
1.2 background tests: each the water base food analogies soak solution and the olive oil soak solution that prepare in 1.1 are operated according to step 2, step 3 and step 4 in the present invention respectively successively, and each practical measurement value of finally calculating gained is listed in table 1, and the mean value and the RSD (relative standard deviation) that calculate practical measurement value are as shown in table 1, this mean value is background values.
The background values determination data (n=6) of parabens material migration amount in table 1 negative sample
The parabens material of 1.3 checkings one, interpolation 10 μ g/kg
Get the polybag drying in 24 1.1, and every 6 one group, in each polybag of first group, all pack in each polybag that all packs 200mL3% acetic acid, the 3rd group in 200mL distilled water, each polybag of second group into, all to pack in 200mL10% ethanol, each polybag of the 4th group and all pack 200g olive oil into, in each polybag, all add 10mg/L parabens standard of physical standard of physical solution 0.2mL afterwards, then according to step 2, step 3 and step 4 in the present invention, operate successively, and calculate recovery rate and RSD as shown in table 2.
In in table 2 negative sample, add the recovery data of the parabens material of 10 μ g/kg
1.4 checkings two, interpolation 100 μ g/kg parabens materials
Get the polybag drying in 24 1.1, and every 6 one group, in each polybag of first group, all pack in each polybag that all packs 200mL3% acetic acid, the 3rd group in 200mL distilled water, each polybag of second group into, all to pack in 200mL 10% ethanol, each polybag of the 4th group and all pack 200g olive oil into, in each polybag, all add 10mg/L parabens standard of physical standard of physical solution 2mL afterwards, then according to step 2, step 3 and step 4 in the present invention, operate successively, and calculate recovery rate and RSD as shown in table 3.
In table 3 negative sample, add the recovery data of the parabens material of 100 μ g/kg
1.5 checkings three, interpolation 200 μ g/kg parabens materials
Get the polybag drying in 24 1.1, and every 6 one group, in each polybag of first group, all pack in each polybag that all packs 200mL3% acetic acid, the 3rd group in 200mL distilled water, each polybag of second group into, all to pack in 200mL10% ethanol, each polybag of the 4th group and all pack 200g olive oil into, in each polybag, all add 10mg/L parabens standard of physical standard of physical solution 4mL afterwards, then according to step 2, step 3 and step 4 in the present invention, operate successively, and calculate recovery rate and RSD as shown in table 4.
In table 4 negative sample, add the recovery data of the parabens material of 200 μ g/kg
Embodiment bis-: testing sample---positive plastic packing bag (positive)
2.1 sample preparations: choose the positive plastic food packing material plastic food packing material of parabens material (containing) and be made into the polybag of 10cm * 10cm with plastic sealing machine, clean with distilled water, dry; Get four these polybags after drying, and be labeled as respectively polybag I, polybag II, polybag III, polybag IV, in polybag I, polybag II, polybag III, be respectively charged into 200mL distilled water, 200mL3% acetic acid, 200mL10% ethanol, and in polybag IV, pack 200g olive oil into; Then with capper, seal each polybag to obtain respectively each water base food analogies soak solution and olive oil soak solution;
2.2 background tests: each the water base food analogies soak solution and the olive oil soak solution that prepare in 2.1 are operated according to step 2, step 3 and step 4 in the present invention respectively successively, and each practical measurement value of finally calculating gained is listed in table 5, and the mean value and the RSD (relative standard deviation) that calculate practical measurement value are as shown in table 5, this mean value is background values.
The background of parabens material migration quantitative determination data in table 5 positive
2.3 checkings one, interpolation 200 μ g/kg parabens materials
Get the polybag drying in 24 2.1, and every 6 one group, in each polybag of first group, all pack 200mL distilled water into, in each polybag of second group, all pack 200mL3% acetic acid into, in each polybag of the 3rd group, all pack 200mL10% ethanol into, in each polybag of the 4th group, all pack 200g olive oil into, in each polybag, all add 10mg/L parabens standard of physical standard of physical solution 4mL afterwards, then successively according to step 2 in the present invention, step 3 and step 4 operate, and calculate recovery of each group and RSD respectively as table 6.1, table 6.2, table 6.3, and shown in table 6.4.
In table 6.1 distilled water immersion liquid, add the recovery data of 200 μ g/kg parabens materials
Object | Measured value (mg/kg) | After button background values (mg/kg) | RSD% |
Methyl hydroxybenzoate | 1.43 | 1.23 | 3.45 |
Ethylparaben | 1.25 | 1.05 | 3.94 |
Propylben | 1.19 | 0.99 | 4.03 |
Nipalgin isopropyl ester | 1.16 | 0.96 | 4.38 |
Nipalgin isobutyl ester | 1.43 | 1.23 | 3.62 |
Butyl hydroxybenzoate | 1.13 | 0.93 | 2.98 |
Heptyl paraben | 1.06 | 0.86 | 3.06 |
Nipalgin monooctyl ester | 1.32 | 1.12 | 3.58 |
In table 6.2 3% acetic acid soak solution, add the recovery data of 200 μ g/kg parabens materials
Object | Measured value (mg/kg) | After button background values (mg/kg) | RSD% |
Methyl hydroxybenzoate | 2.09 | 1.89 | 3.21 |
Ethylparaben | 1.97 | 1.77 | 3.51 |
Propylben | 1.88 | 1.68 | 2.68 |
Nipalgin isopropyl ester | 2.13 | 1.93 | 3.06 |
Nipalgin isobutyl ester | 2.11 | 1.91 | 2.65 |
Butyl hydroxybenzoate | 1.71 | 1.51 | 2.81 |
Heptyl paraben | 1.62 | 1.42 | 2.91 |
Nipalgin monooctyl ester | 1.83 | 1.63 | 3.09 |
In table 6.3 10% alcohol immersion liquid, add the recovery data of 200 μ g/kg parabens materials
Object | Measured value (mg/kg) | After button background values (mg/kg) | RSD% |
Methyl hydroxybenzoate | 1.99 | 1.79 | 2.38 |
Ethylparaben | 1.91 | 1.71 | 2.91 |
Propylben | 1.84 | 1.64 | 2.62 |
Nipalgin isopropyl ester | 2.15 | 1.95 | 2.09 |
Nipalgin isobutyl ester | 2.05 | 1.85 | 3.02 |
Butyl hydroxybenzoate | 1.78 | 1.58 | 1.99 |
Heptyl paraben | 1.73 | 1.53 | 2.03 |
Nipalgin monooctyl ester | 1.92 | 1.72 | 2.67 |
In table 6.4 olive oil soak solution, add the recovery data of 200 μ g/kg parabens materials
Object | Measured value (mg/kg) | After button background values (mg/kg) | RSD% |
Methyl hydroxybenzoate | 1.54 | 1.34 | 4.62 |
Ethylparaben | 1.21 | 1.01 | 4.03 |
Propylben | 1.46 | 1.26 | 3.99 |
Nipalgin isopropyl ester | 1.39 | 1.19 | 3.68 |
Nipalgin isobutyl ester | 1.44 | 1.24 | 4.54 |
Butyl hydroxybenzoate | 1.31 | 1.11 | 4.31 |
Heptyl paraben | 1.21 | 1.01 | 3.26 |
Nipalgin monooctyl ester | 1.50 | 1.30 | 4.01 |
Checking in the various embodiments described above is known, when detection method of the present invention is applied to detect the migration amount of parabens material in plastic packing bag, it is not only feasible that the large I of the recovery from the result separately and RSD is judged detection method of the present invention, and accuracy is high.
In addition, although the present invention sets forth exposure with above-described embodiment, it has and conventionally knows the knowledgeable in any affiliated technical field not in order to limit the present invention, all equalizations according to doing within the scope of the present patent application claim change and retouching, all should belong to scope of the present invention.
Claims (2)
1. a detection method for parabens material migration amount in plastic packing bag, is characterized in that: it specifically comprises following operation steps:
Step 1, sample preparation: choose plastic sample and with plastic sealing machine, be made into the polybag of 10cm * 10cm, with distilled water, clean, dry; Get this polybag after drying and pack the water base food simulated solution of 200mL into, then get this polybag after drying and pack 200g olive oil into, then with capper sealing to obtain respectively water base food analogies soak solution and olive oil soak solution;
Step 2, sample purification:
(1) oil base food analogies: get the olive oil soak solution 0.5g that step 1 obtains, and add 3mL isooctane to dissolve, vortex 2min mixes to obtain mixed liquor, then mixed liquor is passed through to C
18post, with 6mL isooctane drip washing pillar and discard efflux, use again 9mL eluent ethyl acetate, collect eluent ethyl acetate liquid and be placed in nitrogen bottle blowing, then at 45 ℃, with nitrogen, liquid in nitrogen bottle blowing is dried up to obtain to residue, this residue is dissolved and the centrifugal 2min of 2500r/min with 1mL methyl alcohol, after centrifugal end, get supernatant and cross 0.22 μ m miillpore filter and obtain filtrate, obtain the liquid to be measured of oil base food analogies;
(2) water base food analogies: the water base food analogies soak solution 1mL that draws step 1 acquisition crosses 0.22 μ m miillpore filter and obtains filtrate, obtains the liquid to be measured of water base food analogies;
Step 3, analyzing and testing: all adopt HPLC/MS/MS to carry out analyzing and testing each liquid to be measured obtaining, particularly, it is the response signal of parabens material to obtain measured object in liquid to be measured that liquid to be measured is carried out to upper machine analysis, according to the response signal of measured object in liquid to be measured, choose the corresponding standard operation liquid of response afterwards and carry out stratographic analysis, standard operation liquid is provided with and comprises zero point in six interior concentration gradients, and in standard operation liquid and liquid to be measured, the response of parabens material all should be in instrument linear response range, and a blank is set simultaneously;
Wherein, the HPLC condition in described HPLC/MS/MS is:
A chromatographic column: ZORBAX SB-C
18, 4.6mm * 150mm, granularity 5 μ m;
B mobile phase: methyl alcohol, water;
C gradient:
D sample size: 5 μ L;
E column temperature: 35 ℃;
And the MS/MS condition in described HPLC/MS/MS is:
A ' ion gun: Negative electrospray ionization source, multiple-reaction monitoring scan mode;
B ' capillary voltage: 4kV;
C ' ion source temperature: 350 ℃;
D ' atomizer pressure: 40psi;
E ' dry gas flow velocity: 8L/min;
The mass spectrum parameter optimization of 8 kinds of nipagin esters of f ':
And being wherein with ★ is quota ion;
Step 4, testing result are calculated: HPLC/MS/MS is obtained to each parameter value substitution following formula (1) or formula (2) is calculated, to obtain the practical measurement value of parabens material in each liquid to be measured;
The migration amount of parabens material in the liquid to be measured of water base food analogies, by following formula (1), calculate:
In formula (1):
The migration amount of parabens material in X-liquid to be measured, unit is mg/kg;
The peak area of parabens material in A-liquid to be measured;
A
0the peak area of parabens material in-blank;
The peak area of parabens material in As-standard operation liquid;
The concentration of parabens material in c-standard operation liquid, unit is mg/L;
V-soak solution volume, unit is L;
The contact area of S-sample and oil base food analogies, unit is dm
2;
In 6-european union directive 2002/72/EC, stipulate mg/kg=6mg/dm
2;
The migration amount of nipagin esters in the liquid to be measured of oil base food analogies, by formula (2), calculate:
In formula (2):
The migration amount of parabens material in X-liquid to be measured, unit is mg/kg;
The peak area of parabens material in A-liquid to be measured;
A
0the peak area of parabens material in-blank;
The peak area of parabens material in As-standard operation liquid;
The concentration of parabens material in c-standard operation liquid, unit is mg/L;
During m-purification, take the quality of olive oil soak solution, unit is kg;
Constant volume after V-olive oil sample purification, unit is L.
2. the detection method of parabens material migration amount in plastic packing bag according to claim 1, is characterized in that: described water base food simulated solution is distilled water, 3% acetic acid or 10% ethanol; And wherein number percent is percent by volume.
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