CN109975441A - The measuring method of volatility and semi-volatile organic matter migration in a kind of canned packaging material - Google Patents
The measuring method of volatility and semi-volatile organic matter migration in a kind of canned packaging material Download PDFInfo
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- CN109975441A CN109975441A CN201711458108.5A CN201711458108A CN109975441A CN 109975441 A CN109975441 A CN 109975441A CN 201711458108 A CN201711458108 A CN 201711458108A CN 109975441 A CN109975441 A CN 109975441A
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- G—PHYSICS
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- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
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Abstract
The present invention provides the measuring method of volatility and semi-volatile organic matter migration in a kind of canned packaging material, includes the following steps: that Migration Simulation object 1) is placed in closed preservation in canned packaging and simulates migration；2) it takes out the Migration Simulation object that step 1) obtains and is fixed in thermal desorption pipe, volatility and semi-volatile organic matter are analyzed using thermal desorption-gas chromatography-mass spectrum.The present invention directly analyzes Migration Simulation object using thermal desorption-gas chromatography-mass spectrum, reduces multistep pre-treatment step, treatment effeciency is high, saves the time, while reducing the introducing of pollutant in solvent and environment, environmentally friendly；Relative to solvent processing method, high sensitivity can carry out screening, qualitative to unknown volatility, semi-volatile organic matter in canned packaging material, while can carry out quantitative analysis to specific volatile, semi-volatile organic matter.
Description
Technical field
The present invention relates to the measuring methods that volatility in canned packaging material and semi-volatile organic matter migrate, and in particular to
A kind of canned measuring method for packing volatility and semi-volatile organic matter migration in inner layer material.
Background technique
Canned packaging has many advantages, such as that satisfactory mechanical property, barrier property are excellent, decoration is exquisite, various shapes, commonly used
In biscuit, tealeaves, coffee, candy, tobacco product packaging.Epoxy resin or vinyl organosol are generallyd use in canned packaging
Interlayer coatings are done, to avoid the corrosion of can internal layer and digestion of metallic ion to cause to pack interior contamination of products.Canned packaging
Interlayer coatings are contacted with product for a long time, and part harmful substance is migrated to be caused to damage into product to human body, there is overpowering odor
Organic matter produces bigger effect product quality.
Safety evaluatio is carried out to canned material and generallys use the canned inner layer material of solvent extraction, in Test extraction object at
Point, this method directly evaluates the safety of canned material, cannot reflect influence of the canned material to product；Directly connect to canned packet
Product is tested in filling, and it is complicated that there are product matrix, and analysis method is complicated, and detection difficulty is big.
Summary of the invention
In view of the foregoing deficiencies of prior art, the present invention provides volatility in the highly sensitive canned packaging material of one kind
With the measuring method of semi-volatile organic matter migration, it is placed directly in canned packaging using Migration Simulation object, in certain condition
Lower sealed storage, volatilization and half volatile matter are migrated analogies absorption in canned packaging inner layer material, and Migration Simulation object is as warm
One kind of adsorbent is desorbed, can directly be seated in progress GC-MS analysis in thermal desorption pipe.After simulating migration, it will move
It moves analogies to be loaded into thermal desorption pipe, directly progress thermal desorption analysis.The thermal desorption pipe for filling Migration Simulation object uses gas phase
Chromatography packed column injection port-autosampler adds internal standard.Measuring method operating procedure of the invention is easy, and treatment effeciency is high,
Volatility, semi-volatile organic matter loss are reduced, avoids pollution the introducing of object, mark-on mode is more reasonable, method high sensitivity, can
Screening, qualitative is carried out to volatility unknown in canned material, semi-volatile organic matter, while can be volatilized to specific volatile, half
Property organic matter carry out quantitative analysis.
In order to solve the above technical problems, the present invention is achieved by the following technical solutions:
The measuring method of volatility and semi-volatile organic matter migration, includes the following steps: in a kind of canned packaging material
1) Migration Simulation object is placed in closed preservation in canned packaging and simulates migration；
2) it takes out the Migration Simulation object that step 1) obtains and is fixed in thermal desorption pipe, using thermal desorption-gas-chromatography-matter
Spectrum analyzes volatility and semi-volatile organic matter:
Qualitative analysis: thermal desorption-gas chromatography-mass spectrum figure is compareed with mass spectrometry database, and analysis obtains canned packing timber
The type of volatility and semi-volatile organic matter in material；
Quantitative analysis: selection criteria substance establishes standard curve, obtains volatility and half volatile in canned packaging material
The amount of migration of organic matter.
Preferably, in step 1), Migration Simulation object is polyphenylene oxide.
Preferably, in step 1), the quality of Migration Simulation object is 0.1~10g.
Preferably, in step 1), simulation migration temperature is room temperature~100 DEG C.
Preferably, in step 1), simulation transit time is 5min~240h.
Preferably, in step 2), the quality for taking out the Migration Simulation object that step 1) obtains is 20~200mg.
Preferably, in step 2), using the fixed polyphenylene oxide of gas phase silica wool in thermal desorption pipe.
Preferably, in step 2), thermal desorption pipe is mounted on gas-chromatography packed column injection port, quantitative using autosampler
Internal standard and standard items are added.The standard items of addition are after injection port vaporization, and the MPPO being adsorbed in thermal desorption pipe, it is qualitative fixed to carry out
Amount.
It is highly preferred that mark-on condition is as follows:
1) packed column injector temperature is 100~250 DEG C；
2) injection port flow is 20~200ml/min；
3) gas chromatographic column Temperature of Warm Case is 35~80 DEG C；
4) standard specimen adsorption time is 1~10min after autosampler mark-on.
Preferably, further include one or more in following technical characteristic in step 2):
1) thermal desorption pipe desorption temperature is 250~350 DEG C；
2) thermal desorption pipe desorption time is 2~60min；
3) adsorption trap adsorption temp is -40~50 DEG C；
4) adsorption trap desorption temperature is 250~350 DEG C；
5) adsorption trap desorption time is 2~60min；
6) desorption flow is 30-80mL/min.
Preferably, closed preservation in canned packaging is placed in after polyphenylene oxide purification again and simulates migration, the purification are as follows: polyphenyl
Ether acetone reflux in Soxhlet extraction device extracts, and is placed in culture dish the acetone that volatilizees, is then toasted in an oven.
It is highly preferred that further including one in following technical characteristic or two:
1) reflux extracting time is 4~8h；
2) baking temperature is 120~200 DEG C, and baking time is 4~8h.
Beneficial effects of the present invention: the survey of volatility and semi-volatile organic matter migration in canned packaging material of the invention
Determine method, directly Migration Simulation object is analyzed using thermal desorption-gas chromatography-mass spectrum.Migration Simulation object is directly carried out
Analysis reduces multistep pre-treatment step, and treatment effeciency is high, saves the time, while reducing the introducing of pollutant in solvent and environment；
The use of organic solvent is reduced, it is environmentally friendly；For method relative to solvent processing method, high sensitivity can be in canned material
Unknown volatility, semi-volatile organic matter carry out screening, qualitative, while can carry out to specific volatile, semi-volatile organic matter
Quantitative analysis.
Detailed description of the invention
Fig. 1 is canned material MPPO simulation migration thermal desorption-gas chromatography-mass spectrum figure in embodiment 1；When abscissa is
Between, unit is minute；Ordinate is signal strength；Analysis show that volatility in canned material, semi-volatile organic matter are mainly
Low boiling point alcohols, ethers.
Fig. 2 is that 2 Plays substance of embodiment selects ion ion detection chromatogram.
Specific embodiment
The present invention is further explained combined with specific embodiments below, it should be appreciated that these embodiments are merely to illustrate the present invention
Rather than it limits the scope of the invention.
Illustrate embodiments of the present invention below by way of specific specific example, those skilled in the art can be by this specification
Other advantages and efficacy of the present invention can be easily understood for disclosed content.The present invention can also pass through in addition different specific realities
The mode of applying is embodied or practiced, the various details in this specification can also based on different viewpoints and application, without departing from
Various modifications or alterations are carried out under spirit of the invention.
Embodiment 1
Polyphenylene oxide acetone reflux in Soxhlet extraction device extracts, and reflux extracting time 8h is placed in culture dish and waves
Acetone is sent out, is then toasted in an oven, baking temperature is 200 DEG C, and baking time 4h obtains the MPPO for the treatment of and purification.
The measuring method of volatility and semi-volatile organic matter migration, includes the following steps: in a kind of canned packaging material
1) MPPO of 0.2g treatment and purification is placed in closed preservation in canned packaging and simulates migration, places 72h at 40 DEG C；
2) after migrating, whole MPPO are fixed in thermal desorption pipe, using thermal desorption-gas chromatography-mass spectrum to waving
Hair property and semi-volatile organic matter are analyzed.
1ul internal standard (0.5ug/mL propyl benzoate) is added in thermal desorption pipe, mark-on condition is as follows:
Packed column injector temperature is 180 DEG C, carrier gas flux 120mL/min, and column oven temperature is 50 DEG C, standard specimen absorption
Time 8min；
350 thermal desorption instrument of platinum Ai Ermo TurboMatrix:
Level-one is desorbed 280 DEG C, desorption time 10min；Flow 40mL/min is desorbed；- 30 DEG C of adsorption trap temperature；Second level desorption
Temperature: 270 DEG C, desorption time 8min；Chromatography column pressure 10psi；
Agilent 7890C, 5975C gas chromatograph-mass spectrometer:
Chromatographic condition: chromatographic column: Vocol (60m × 0.32mm, 1.8um)；Carrier gas: He；Temperature programming: initial temperature 35
DEG C, it maintains 10min, 3.5 DEG C/min to be warming up to 180 DEG C, continues to be warming up to 210 DEG C with 10 DEG C/min, maintain 5min.
Mass Spectrometry Conditions: ion source: EI；Ionization energy: 70eV；Ion source temperature: 230 DEG C；Level four bars temperature: 150 DEG C；Solvent
Delay: 3min；Detection pattern: full scan detects (SCAN).
As shown in Figure 1, by compareing with NIST mass spectrometry database, analysis obtains canned thermal desorption-gas chromatography-mass spectrum figure
Volatility, semi-volatile organic matter are mainly low boiling point alcohols, ethers in material.
Embodiment 2
Polyphenylene oxide acetone reflux in Soxhlet extraction device extracts, and reflux extracting time 8h is placed in culture dish and waves
Acetone is sent out, is then toasted in an oven, baking temperature is 200 DEG C, and baking time 4h obtains the MPPO for the treatment of and purification.
1) MPPO of 0.15g treatment and purification is placed in closed preservation in canned packaging and simulates migration, places 72h at 40 DEG C；
2) after migrating, whole MPPO are fixed in thermal desorption pipe, using thermal desorption-gas chromatography-mass spectrum to waving
Hair property and semi-volatile organic matter are analyzed.
1ul internal standard (0.5ug/mL propyl benzoate) and 1ul various concentration esters of acrylic acid are separately added into thermal desorption pipe
Standard specimen (0.1ug/ml, 0.2ug/ml, 0.5ug/ml, 1ug/ml, 2ug/ml, 5ug/ml), supervises acrylate substance
Control, while investigating the quantitative limit, detection limit, repeatability and the rate of recovery of this method.Mark-on instrument condition is as follows:
Packed column injector temperature is 150 DEG C, carrier gas flux 100mL/min, and column oven temperature is 40 DEG C, standard specimen absorption
Time 5min.
350 thermal desorption instrument of platinum Ai Ermo TurboMatrix:
Level-one is desorbed 280 DEG C, desorption time 10min；Flow 40mL/min is desorbed；- 30 DEG C of adsorption trap temperature；Second level desorption
Temperature: 270 DEG C, desorption time 8min；Chromatography column pressure 10psi；
Agilent 7890C, 5975C gas chromatograph-mass spectrometer:
Chromatographic condition: chromatographic column: Wax (60m × 0.32mm, 1.8um)；Carrier gas: He；Temperature programming: 35 DEG C of initial temperature,
It maintains 10min, 5 DEG C/min to be warming up to 240 DEG C, maintains 10min.
Mass Spectrometry Conditions: ion source: EI；Ionization energy: 70eV；Ion source temperature: 230 DEG C；Level four bars temperature: 150 DEG C；Solvent
Delay: 3min；Detection pattern: selection ion detection (SIM), quantitative and qualitative ion such as table 1.
Acrylic method investigates data such as table 2, and standard substance selects ion ion detection chromatogram such as Fig. 2 institute
Show.
This method high sensitivity, stability can carry out effective monitoring to acrylic in canned material well.
1 acrylic quota ion of table and qualitative ion
| Serial number | Compound name | Retention time/min | Quota ion | Qualitative ion |
| 1 | Methyl acrylate | 7.38 | 55 | 85 |
| 2 | Ethyl acrylate | 9.67 | 55 | 99 |
| 3 | Methyl methacrylate | 10.24 | 69 | 100 |
| 4 | Ethyl methacrylate | 12.56 | 69 | 41 |
| 5 | Isobutyl methacrylate | 18.03 | 69 | 87 |
| 6 | Butyl acrylate | 18.36 | 55 | 73 |
| 7 | N-BMA | 20.31 | 69 | 87 |
| 8 | Propyl benzoate IS | 34.79 | 105 | 77 |
2 acrylic method of table investigates data
The above-described embodiments merely illustrate the principles and effects of the present invention, and is not intended to limit the present invention.It is any ripe
The personage for knowing this technology all without departing from the spirit and scope of the present invention, carries out modifications and changes to above-described embodiment.Cause
This, institute is complete without departing from the spirit and technical ideas disclosed in the present invention by those of ordinary skill in the art such as
At all equivalent modifications or change, should be covered by the claims of the present invention.
Claims (12)
1. the measuring method of volatility and semi-volatile organic matter migration in a kind of canned packaging material, which is characterized in that including
Following steps:
1) Migration Simulation object is placed in closed preservation in canned packaging and simulates migration；
2) it takes out the Migration Simulation object that step 1) obtains and is fixed in thermal desorption pipe, using thermal desorption-gas chromatography-mass spectrum pair
Volatility and semi-volatile organic matter are analyzed:
Qualitative analysis: thermal desorption-gas chromatography-mass spectrum figure is compareed with mass spectrometry database, and analysis obtains in canned packaging material
The type of volatility and semi-volatile organic matter；
Quantitative analysis: selection criteria substance establishes standard curve, show that volatility and half volatile are organic in canned packaging material
The amount of migration of object.
2. measuring method as described in claim 1, which is characterized in that in step 1), Migration Simulation object is polyphenylene oxide.
3. measuring method as described in claim 1, which is characterized in that in step 1), the quality of Migration Simulation object is 0.1~
10g。
4. measuring method as described in claim 1, which is characterized in that in step 1), simulation migration temperature is room temperature~100
℃。
5. measuring method as described in claim 1, which is characterized in that in step 1), simulation transit time is 5min~240h.
6. measuring method as described in claim 1, which is characterized in that in step 2), take out the Migration Simulation that step 1) obtains
The quality of object is 20~200mg.
7. measuring method as described in claim 1, which is characterized in that in step 2), using the fixed polyphenylene oxide of gas phase silica wool
In thermal desorption pipe.
8. measuring method as described in claim 1, which is characterized in that in step 2), thermal desorption pipe is mounted on gas-chromatography and fills out
Column injection port is filled, internal standard and standard items are quantitatively adding using autosampler.
9. measuring method as claimed in claim 8, which is characterized in that mark-on condition is as follows:
1) packed column injector temperature is 100~250 DEG C；
2) injection port flow is 20~200ml/min；
3) gas chromatographic column Temperature of Warm Case is 35~80 DEG C；
4) standard specimen adsorption time is 1~10min after autosampler mark-on.
10. measuring method as described in claim 1, which is characterized in that further include one in following technical characteristic in step 2)
Item is multinomial:
1) thermal desorption pipe desorption temperature is 250~350 DEG C；
2) thermal desorption pipe desorption time is 2~60min；
3) adsorption trap adsorption temp is -40~50 DEG C；
4) adsorption trap desorption temperature is 250~350 DEG C；
5) adsorption trap desorption time is 2~60min；
6) desorption flow is 30-80mL/min.
11. measuring method as described in claim 1, which is characterized in that be placed in again after polyphenylene oxide purification closed in canned packaging
Save and simulate migration, the purification are as follows: polyphenylene oxide acetone reflux in Soxhlet extraction device extracts, and is placed in culture dish and waves
Acetone is sent out, is then toasted in an oven.
12. measuring method as claimed in claim 11, which is characterized in that further include one or two in following technical characteristic
:
1) reflux extracting time is 4~8h；
2) baking temperature is 120~200 DEG C, and baking time is 4~8h.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN112924595A (en) * | 2021-01-27 | 2021-06-08 | 上海烟草集团有限责任公司 | Method for detecting acrylic resin monomer migration volume in paper packaging material |
| CN113030299A (en) * | 2021-02-22 | 2021-06-25 | 广州海关技术中心 | Method for screening and evaluating safety of unintended or intended additive migration amount in recycled PET (polyethylene terephthalate) product for food contact |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112924595A (en) * | 2021-01-27 | 2021-06-08 | 上海烟草集团有限责任公司 | Method for detecting acrylic resin monomer migration volume in paper packaging material |
| CN113030299A (en) * | 2021-02-22 | 2021-06-25 | 广州海关技术中心 | Method for screening and evaluating safety of unintended or intended additive migration amount in recycled PET (polyethylene terephthalate) product for food contact |
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