CN111624290A - Method for determining VOCs in packaging material by purging and trapping-gas chromatography-mass spectrometry - Google Patents
Method for determining VOCs in packaging material by purging and trapping-gas chromatography-mass spectrometry Download PDFInfo
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- CN111624290A CN111624290A CN202010390047.9A CN202010390047A CN111624290A CN 111624290 A CN111624290 A CN 111624290A CN 202010390047 A CN202010390047 A CN 202010390047A CN 111624290 A CN111624290 A CN 111624290A
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- 238000010926 purge Methods 0.000 title claims abstract description 26
- 238000000034 method Methods 0.000 title claims abstract description 21
- 239000005022 packaging material Substances 0.000 title claims abstract description 21
- 238000002290 gas chromatography-mass spectrometry Methods 0.000 title claims abstract description 11
- 239000012855 volatile organic compound Substances 0.000 title claims description 21
- 239000002904 solvent Substances 0.000 claims abstract description 9
- 238000004949 mass spectrometry Methods 0.000 claims abstract description 8
- 238000005070 sampling Methods 0.000 claims abstract description 6
- 238000012790 confirmation Methods 0.000 claims abstract description 4
- 238000004445 quantitative analysis Methods 0.000 claims abstract description 4
- 238000002360 preparation method Methods 0.000 claims abstract description 3
- 239000000523 sample Substances 0.000 claims description 45
- 239000000126 substance Substances 0.000 claims description 9
- 239000007789 gas Substances 0.000 claims description 8
- 230000004044 response Effects 0.000 claims description 7
- 238000002347 injection Methods 0.000 claims description 6
- 239000007924 injection Substances 0.000 claims description 6
- 238000007664 blowing Methods 0.000 claims description 5
- 239000012491 analyte Substances 0.000 claims description 3
- 239000012159 carrier gas Substances 0.000 claims description 3
- 238000003795 desorption Methods 0.000 claims description 3
- 239000001307 helium Substances 0.000 claims description 3
- 229910052734 helium Inorganic materials 0.000 claims description 3
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 claims description 3
- 238000012417 linear regression Methods 0.000 claims description 3
- 230000014759 maintenance of location Effects 0.000 claims description 3
- 238000001819 mass spectrum Methods 0.000 claims description 3
- 239000013557 residual solvent Substances 0.000 claims description 3
- 239000012488 sample solution Substances 0.000 claims description 3
- 239000000243 solution Substances 0.000 claims description 3
- 238000005520 cutting process Methods 0.000 claims description 2
- 238000007789 sealing Methods 0.000 claims description 2
- 238000012360 testing method Methods 0.000 abstract description 8
- 238000001514 detection method Methods 0.000 abstract description 5
- 150000002148 esters Chemical class 0.000 abstract description 4
- 150000001298 alcohols Chemical class 0.000 abstract description 3
- 150000002576 ketones Chemical class 0.000 abstract description 3
- 238000010408 sweeping Methods 0.000 abstract description 3
- 150000001335 aliphatic alkanes Chemical class 0.000 abstract description 2
- 238000004458 analytical method Methods 0.000 abstract description 2
- 150000001555 benzenes Chemical class 0.000 abstract description 2
- 238000000605 extraction Methods 0.000 abstract description 2
- 238000004817 gas chromatography Methods 0.000 abstract description 2
- 150000008282 halocarbons Chemical class 0.000 abstract description 2
- 239000003960 organic solvent Substances 0.000 abstract description 2
- 239000002957 persistent organic pollutant Substances 0.000 abstract description 2
- 230000035945 sensitivity Effects 0.000 abstract description 2
- 238000004364 calculation method Methods 0.000 abstract 1
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 6
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 description 3
- 230000007547 defect Effects 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 150000001336 alkenes Chemical class 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000005003 food packaging material Substances 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 239000000976 ink Substances 0.000 description 1
- JMMWKPVZQRWMSS-UHFFFAOYSA-N isopropyl acetate Chemical compound CC(C)OC(C)=O JMMWKPVZQRWMSS-UHFFFAOYSA-N 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000002414 normal-phase solid-phase extraction Methods 0.000 description 1
- 238000004806 packaging method and process Methods 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 238000002203 pretreatment Methods 0.000 description 1
- 230000002265 prevention Effects 0.000 description 1
- 238000011002 quantification Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000002470 solid-phase micro-extraction Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- 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
- G01N30/02—Column chromatography
- G01N30/88—Integrated analysis systems specially adapted therefor, not covered by a single one of the groups G01N30/04 - G01N30/86
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- 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
- G01N30/02—Column chromatography
- G01N30/88—Integrated analysis systems specially adapted therefor, not covered by a single one of the groups G01N30/04 - G01N30/86
- G01N2030/8809—Integrated analysis systems specially adapted therefor, not covered by a single one of the groups G01N30/04 - G01N30/86 analysis specially adapted for the sample
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- 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
- G01N30/02—Column chromatography
- G01N30/88—Integrated analysis systems specially adapted therefor, not covered by a single one of the groups G01N30/04 - G01N30/86
- G01N2030/8809—Integrated analysis systems specially adapted therefor, not covered by a single one of the groups G01N30/04 - G01N30/86 analysis specially adapted for the sample
- G01N2030/884—Integrated analysis systems specially adapted therefor, not covered by a single one of the groups G01N30/04 - G01N30/86 analysis specially adapted for the sample organic compounds
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- 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
- G01N30/02—Column chromatography
- G01N30/88—Integrated analysis systems specially adapted therefor, not covered by a single one of the groups G01N30/04 - G01N30/86
- G01N2030/8809—Integrated analysis systems specially adapted therefor, not covered by a single one of the groups G01N30/04 - G01N30/86 analysis specially adapted for the sample
- G01N2030/884—Integrated analysis systems specially adapted therefor, not covered by a single one of the groups G01N30/04 - G01N30/86 analysis specially adapted for the sample organic compounds
- G01N2030/8854—Integrated analysis systems specially adapted therefor, not covered by a single one of the groups G01N30/04 - G01N30/86 analysis specially adapted for the sample organic compounds involving hydrocarbons
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- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
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Abstract
The invention relates to a method for determining VOCs in a packaging material by sweeping, trapping, gas chromatography and mass spectrometry, which is characterized by comprising the following steps: the method comprises the steps of sample preparation, purging, trapping and sample introduction, chromatography-mass spectrometry combined determination, qualitative confirmation, quantitative analysis and calculation result analysis. The method for determining the VOCs in the packaging material by the purging trapping-gas chromatography-mass spectrometry has the advantages that the structural design is scientific and reasonable, and the content of 25 volatile organic pollutants (VOCs) in the packaging material and products can be determined; a sweeping, trapping and sampling mode is adopted, so that the extraction and concentration of an organic solvent are avoided, and the interference of an external solvent is reduced; the sample area required by purging and trapping is small compared with that of a headspace, the sensitivity is high, the gas chromatography-mass spectrometer is used for detection, the qualitative capability of the method is enhanced, and the false positive risk is reduced; the test types of patents are more, and the test types comprise alcohols, esters, ketones, benzenes, alkane, halogenated hydrocarbons and the like, and the test requirements on VOCs in the packaging material at present are basically met.
Description
Technical Field
The invention belongs to the technical field of packaging material detection, relates to determination of VOCs in packaging materials, and particularly relates to a method for determining VOCs in packaging materials by purge trapping-gas chromatography-mass spectrometry.
Background
At present, raw materials (including but not limited to inks, solvents, polymers, etc.) used in the production and printing of packaging materials contain a large amount of Volatile Organic Compounds (VOCs) including alcohols, ketones, alkenes, esters, benzene, and benzene-based esters, and these packaging materials may migrate into food, medical supplies or environments during use, causing harm to human health, so an analysis method for simultaneously measuring a plurality of volatile organic compounds in the packaging materials is needed.
At the present stage, a headspace method and a solid phase microextraction method are mainly adopted for pretreatment of VOCs detection, the headspace method is large in sampling area, and pretreatment is required for a sample to extract gas; solid phase extraction also requires pre-treatment of the sample to obtain the extract. This results in a loss of the substance to be tested in the sample and also increases the interference factor. Although the gas chromatography used at present can meet the detection and prevention and control requirements in terms of quantification, the defects of inaccuracy and narrow coverage range exist in the qualitative determination of chemicals, and improvement is needed.
Disclosure of Invention
The invention aims to provide a method for determining VOCs in a packaging material by purging and trapping-gas chromatography-mass spectrometry, aiming at the defects and shortcomings of the prior art, so that the external interference can be reduced, and the qualitative capability of each substance in the VOCs can be improved; meanwhile, the determination types can be increased, and the test requirements in different fields can be met.
The technical problem to be solved by the invention is realized by the following technical scheme:
a method for determining VOCs in packaging materials by purge trapping-gas chromatography-mass spectrometry is characterized in that: the method comprises the following steps:
1) sample preparation: cutting to 10cm2Placing the sample to be detected in a blowing bottle, and sealing the blowing bottle to be detected;
2) purging, trapping and sampling: sending the sample obtained in the step 1) into a purging and trapping sample injector, wherein the sample injection conditions are as follows: the temperature of the sample cup is 80 ℃, the purging time is 11min, and the desorption temperature is 250 ℃;
3) combined chromatography-mass spectrometry: injecting a sample to be detected into a gas chromatography-mass spectrometer by using a purging and trapping sample injector to perform chromatography-mass spectrometry combined determination;
4) and (3) qualitative confirmation: the chromatographic peak of the sample solution to be detected and the known standard substance appears at the same retention time, and the target analyte can be qualitatively confirmed at the moment;
5) quantitative analysis: taking the volume of each standard substance solution as an abscissa and the quantitative chromatographic response value of the grid as an ordinate, making a linear regression direction of a standard curve, and comparing and quantifying the response value of the sample with the standard curve;
6) and (3) calculating the result: the solvent residual amount was calculated according to the following formula (1):
wherein:
w is the residual solvent amount in milligrams per square meter (mg/m)2)；
P is the corresponding amount in milligrams (mg);
s is the area, mass or volume of the sample in square meters (m)2)。
Moreover, the chromatographic conditions in the step 3) are as follows: DB-624(30m × 0.32mm × 1.8 μm) capillary chromatographic column with high-purity helium as carrier gas, and having split-flow sample injection, split-flow ratio of 10:1, gas flow rate of 1.5mL/min, initial column temperature of 35 deg.C, 1min holding, 5 deg.C/min raising to 180 deg.C holding for 1min, sample inlet temperature of 220 deg.C, interface temperature of 240 deg.C, and solvent delay of 2 min.
Moreover, the mass spectrum conditions in the step 3) are as follows: ion source temperature 230 ℃, quadrupole rod temperature 150 ℃, ionization mode: EI, ionization energy: 70eV, a mass scanning range of 30-450 amu, a SIM scanning mode as a measuring mode and standard spectrogram tuning.
The invention has the advantages and beneficial effects that:
1. the method for determining VOCs in the packaging material by purging and trapping-gas chromatography-mass spectrometry can determine the content of 25 volatile organic pollutants (VOCs) in the packaging material and products; firstly, a sweeping, trapping and sampling mode is adopted, so that the extraction and concentration by using an organic solvent are avoided, and the interference of an external solvent is reduced; the sample area required by purging and trapping is small compared with that of a headspace, the sensitivity is high, and then a gas chromatography-mass spectrometer is used for detection, so that the qualitative capability of the method is enhanced, and the false positive risk is reduced; and finally, the test types of the patent are more, the patent contains alcohols, esters, ketones, benzenes, alkane, halogenated hydrocarbons and the like, and the test requirements on VOCs in the packaging material at present are basically met.
Drawings
Fig. 1 is a total ion flow diagram of 25 VOCs.
Detailed Description
The present invention is further illustrated by the following specific examples, which are intended to be illustrative, not limiting and are not intended to limit the scope of the invention.
A method for determining VOCs in packaging materials by purge trapping-gas chromatography-mass spectrometry is characterized in that: the method comprises the following steps:
1) preparing a sample, namely preparing a food packaging PAPER and plastic composite film bag, wherein the specification and the model are that the material is BOPET/PAPER/PE, the size (mm) is 380 × 295 × 0.145.145, the sample is described as a sample, the surface of the sample is sealed and packaged, the sample is printed, and the test content is that the food packaging material VOCs is tested, and 10cm of dense areas of printed patterns in the material are cut2A sample to be detected is placed in a blowing bottle and sealed to be detected;
2) purging, trapping and sampling: sending the sample obtained in the step 1) into a purging and trapping sample injector, wherein the sample injection conditions are as follows: the temperature of the sample cup is 80 ℃, the purging time is 11min, and the desorption temperature is 250 ℃;
3) combined chromatography-mass spectrometry: injecting a sample to be detected into a gas chromatography-mass spectrometer by using a purging and trapping sample injector to perform chromatography-mass spectrometry combined determination;
the chromatographic conditions are as follows: DB-624(30m × 0.32mm × 1.8 μm) capillary chromatographic column with high-purity helium as carrier gas, and having split-flow sample injection, split-flow ratio of 10:1, gas flow rate of 1.5mL/min, initial column temperature of 35 deg.C, 1min holding, 5 deg.C/min raising to 180 deg.C holding for 1min, sample inlet temperature of 220 deg.C, interface temperature of 240 deg.C, and solvent delay of 2 min;
the mass spectrum conditions are as follows: ion source temperature 230 ℃, quadrupole rod temperature 150 ℃, ionization mode: EI, ionization energy: 70eV, a mass scanning range is 30-450 amu, a measuring mode is an SIM scanning mode, and a standard spectrogram is tuned;
4) and (3) qualitative confirmation: the chromatographic peak of the sample solution to be detected and the known standard substance appears at the same retention time, and the target analyte can be qualitatively confirmed at the moment;
TABLE 1 VOCs component quantitative ion Table
5) Quantitative analysis: taking the volume of each standard substance solution as an abscissa and the quantitative chromatographic response value of the grid as an ordinate, making a linear regression direction of a standard curve, and comparing and quantifying the response value of the sample with the standard curve;
calculating the response value of the test sample;
the result calculated by the software was 6.55mg/m ethyl acetate2Isopropyl acetate 0.61mg/m2。
6) And (3) calculating the result: the solvent residual amount was calculated according to the following formula (1):
wherein:
w is the residual solvent amount in milligrams per square meter (mg/m)2)；
P is the corresponding amount in milligrams (mg);
s is the area, mass or volume of the sample in square meters (m)2)。
Although the embodiments of the present invention and the accompanying drawings are disclosed for illustrative purposes, those skilled in the art will appreciate that: various substitutions, changes and modifications are possible without departing from the spirit and scope of the invention and the appended claims, and therefore the scope of the invention is not limited to the disclosure of the embodiments and the accompanying drawings.
Claims (3)
1. A method for determining VOCs in packaging materials by purge trapping-gas chromatography-mass spectrometry is characterized in that: the method comprises the following steps:
1) sample preparation: cutting to 10cm2Placing the sample to be detected in a blowing bottle, and sealing the blowing bottle to be detected;
2) purging, trapping and sampling: sending the sample obtained in the step 1) into a purging and trapping sample injector, wherein the sample injection conditions are as follows: the temperature of the sample cup is 80 ℃, the purging time is 11min, and the desorption temperature is 250 ℃;
3) combined chromatography-mass spectrometry: injecting a sample to be detected into a gas chromatography-mass spectrometer by using a purging and trapping sample injector to perform chromatography-mass spectrometry combined determination;
4) and (3) qualitative confirmation: the chromatographic peak of the sample solution to be detected and the known standard substance appears at the same retention time, and the target analyte can be qualitatively confirmed at the moment;
5) quantitative analysis: taking the volume of each standard substance solution as an abscissa and the quantitative chromatographic response value of the grid as an ordinate, making a linear regression direction of a standard curve, and comparing and quantifying the response value of the sample with the standard curve;
6) and (3) calculating the result: the solvent residual amount was calculated according to the following formula (1):
wherein:
w is the residual solvent amount in milligrams per square meter (mg/m)2)；
P is the corresponding amount in milligrams (mg);
s is the area, mass or volume of the sample in square meters (m)2)。
2. The method of purge trap-gas chromatography-mass spectrometry of claim 1 for the determination of VOCs in packaging materials, wherein: the chromatographic conditions in the step 3) are as follows: DB-624(30m × 0.32mm × 1.8 μm) capillary chromatographic column with high-purity helium as carrier gas, and having split-flow sample injection, split-flow ratio of 10:1, gas flow rate of 1.5mL/min, initial column temperature of 35 deg.C, 1min holding, 5 deg.C/min raising to 180 deg.C holding for 1min, sample inlet temperature of 220 deg.C, interface temperature of 240 deg.C, and solvent delay of 2 min.
3. The method of purge trap-gas chromatography-mass spectrometry of claim 1 for the determination of VOCs in packaging materials, wherein: the mass spectrum conditions in the step 3) are as follows: ion source temperature 230 ℃, quadrupole rod temperature 150 ℃, ionization mode: EI, ionization energy: 70eV, a mass scanning range of 30-450 amu, a SIM scanning mode as a measuring mode and standard spectrogram tuning.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114778720A (en) * | 2022-03-31 | 2022-07-22 | 红塔烟草(集团)有限责任公司 | P & T-GC-MS method for detecting characteristic aroma components in tow flavored filter stick |
| CN115184511A (en) * | 2022-08-25 | 2022-10-14 | 宜宾五粮液股份有限公司 | Method for in-situ determination of volatile phenols in white spirit |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114778720A (en) * | 2022-03-31 | 2022-07-22 | 红塔烟草(集团)有限责任公司 | P & T-GC-MS method for detecting characteristic aroma components in tow flavored filter stick |
| CN115184511A (en) * | 2022-08-25 | 2022-10-14 | 宜宾五粮液股份有限公司 | Method for in-situ determination of volatile phenols in white spirit |
| CN115184511B (en) * | 2022-08-25 | 2023-09-19 | 宜宾五粮液股份有限公司 | Method for in-situ determination of volatile phenolic substances in white spirit |
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