CN110780000A - Method for detecting migration amount of volatile organic compounds in paper packaging material to dry simulant - Google Patents
Method for detecting migration amount of volatile organic compounds in paper packaging material to dry simulant Download PDFInfo
- Publication number
- CN110780000A CN110780000A CN201911058776.8A CN201911058776A CN110780000A CN 110780000 A CN110780000 A CN 110780000A CN 201911058776 A CN201911058776 A CN 201911058776A CN 110780000 A CN110780000 A CN 110780000A
- Authority
- CN
- China
- Prior art keywords
- volatile organic
- organic compounds
- sample
- dry
- simulant
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- 239000012855 volatile organic compound Substances 0.000 title claims abstract description 61
- 238000013508 migration Methods 0.000 title claims abstract description 39
- 230000005012 migration Effects 0.000 title claims abstract description 39
- 238000000034 method Methods 0.000 title claims abstract description 32
- 239000005022 packaging material Substances 0.000 title claims abstract description 19
- 238000010926 purge Methods 0.000 claims abstract description 45
- 238000001514 detection method Methods 0.000 claims abstract description 28
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 claims abstract description 27
- YKYONYBAUNKHLG-UHFFFAOYSA-N propyl acetate Chemical compound CCCOC(C)=O YKYONYBAUNKHLG-UHFFFAOYSA-N 0.000 claims abstract description 26
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 22
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims abstract description 18
- ARXJGSRGQADJSQ-UHFFFAOYSA-N 1-methoxypropan-2-ol Chemical compound COCC(C)O ARXJGSRGQADJSQ-UHFFFAOYSA-N 0.000 claims abstract description 14
- BDERNNFJNOPAEC-UHFFFAOYSA-N propan-1-ol Chemical compound CCCO BDERNNFJNOPAEC-UHFFFAOYSA-N 0.000 claims abstract description 14
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 12
- 239000012224 working solution Substances 0.000 claims abstract description 12
- 239000007864 aqueous solution Substances 0.000 claims abstract description 5
- 238000001926 trapping method Methods 0.000 claims abstract description 5
- 239000007789 gas Substances 0.000 claims description 11
- 238000002290 gas chromatography-mass spectrometry Methods 0.000 claims description 11
- 230000004044 response Effects 0.000 claims description 11
- 238000010438 heat treatment Methods 0.000 claims description 10
- 238000003795 desorption Methods 0.000 claims description 9
- 238000012360 testing method Methods 0.000 claims description 8
- 239000000463 material Substances 0.000 claims description 6
- 239000001307 helium Substances 0.000 claims description 5
- 229910052734 helium Inorganic materials 0.000 claims description 5
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 claims description 5
- 238000004147 desorption mass spectrometry Methods 0.000 claims description 4
- 238000002156 mixing Methods 0.000 claims description 4
- 238000004458 analytical method Methods 0.000 claims description 3
- 238000000642 dynamic headspace extraction Methods 0.000 claims 1
- 230000003278 mimic effect Effects 0.000 claims 1
- 229920001955 polyphenylene ether Polymers 0.000 claims 1
- 230000035945 sensitivity Effects 0.000 abstract description 5
- 239000011550 stock solution Substances 0.000 description 11
- 238000011084 recovery Methods 0.000 description 9
- 230000010355 oscillation Effects 0.000 description 8
- 238000004806 packaging method and process Methods 0.000 description 7
- 239000000126 substance Substances 0.000 description 7
- 230000004888 barrier function Effects 0.000 description 6
- 238000005516 engineering process Methods 0.000 description 6
- 238000005119 centrifugation Methods 0.000 description 5
- 235000013305 food Nutrition 0.000 description 5
- 238000007664 blowing Methods 0.000 description 4
- 238000003988 headspace gas chromatography Methods 0.000 description 4
- 238000004949 mass spectrometry Methods 0.000 description 4
- 239000012086 standard solution Substances 0.000 description 4
- 230000003068 static effect Effects 0.000 description 4
- 238000005303 weighing Methods 0.000 description 4
- 230000008901 benefit Effects 0.000 description 3
- 239000011521 glass Substances 0.000 description 3
- 238000012986 modification Methods 0.000 description 3
- 230000004048 modification Effects 0.000 description 3
- 239000012851 printed packaging material Substances 0.000 description 3
- 239000000741 silica gel Substances 0.000 description 3
- 229910002027 silica gel Inorganic materials 0.000 description 3
- 238000005520 cutting process Methods 0.000 description 2
- 238000000605 extraction Methods 0.000 description 2
- 239000003960 organic solvent Substances 0.000 description 2
- 239000004810 polytetrafluoroethylene Substances 0.000 description 2
- 229920001343 polytetrafluoroethylene Polymers 0.000 description 2
- 238000007639 printing Methods 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 230000007480 spreading Effects 0.000 description 2
- 238000003892 spreading Methods 0.000 description 2
- 238000012546 transfer Methods 0.000 description 2
- 229910021642 ultra pure water Inorganic materials 0.000 description 2
- 239000012498 ultrapure water Substances 0.000 description 2
- 238000013019 agitation Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000007865 diluting Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000004817 gas chromatography Methods 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- -1 low Substances 0.000 description 1
- 238000001819 mass spectrum Methods 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 229920013638 modified polyphenyl ether Polymers 0.000 description 1
- 238000012544 monitoring process Methods 0.000 description 1
- 150000002894 organic compounds Chemical class 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 238000011002 quantification Methods 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000000638 solvent extraction Methods 0.000 description 1
Classifications
-
- 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
-
- 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
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
-
- 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
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
- G01N2030/062—Preparation extracting sample from raw material
Landscapes
- Physics & Mathematics (AREA)
- 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)
- Immunology (AREA)
- Pathology (AREA)
- Other Investigation Or Analysis Of Materials By Electrical Means (AREA)
Abstract
The invention provides a method for detecting the migration amount of volatile organic compounds in a paper packaging material to a dry simulant, wherein a standard sample and a sample to be detected capture the volatile organic compounds by a purging and trapping method respectively, wherein the standard sample is a standard working solution formed by adding a certain amount of the dry simulant into a series of volatile organic compounds with different concentrations respectively; volatile organic compounds include ethanol, isopropanol, n-propanol, ethyl acetate, 1-methoxy-2-propanol and n-propyl acetate; the sample to be measured is an aqueous solution formed by adding the same amount of dry simulant into water after migration treatment is carried out on the dry simulant by adopting a paper packaging material, wherein the volume of the added water is the same as the volume of the added volatile organic compounds when the standard sample is prepared. The method improves the detection sensitivity, and is simple and environment-friendly.
Description
Technical Field
The invention relates to a technology for detecting chemical components in a paper packaging material, in particular to a method for detecting the migration volume of volatile organic compounds in the paper packaging material.
Background
The detection of volatile organic compounds in printed packaging material is of vital importance for monitoring the security of printed packaging material. At present, headspace-gas chromatography/mass spectrometry and the like are mainly used for detecting volatile organic compounds, wherein static headspace-gas chromatography/mass spectrometry is most widely used due to the advantages of small matrix interference, simpler instrument, few false positives and the like. However, some harmful substances in the printed packaging material can be harmful to the health of consumers if the harmful substances migrate into the food even if the content of the harmful substances is trace, and the static headspace-gas chromatography/mass spectrometry has low sensitivity and is not enough to meet the requirements of partial substance migration amount research and detection.
The purging and trapping method belongs to the category of gas phase extraction, organic solvent extraction and concentration are not used, complex pretreatment steps are avoided, interference is less, the method has the advantages of simplicity in operation, low detection limit and the like, research has been conducted on detection of residual quantity of printing materials of printing packages, and compared with a static headspace-gas chromatography/mass spectrometry method, the sensitivity is remarkably improved. However, the residual quantity detection is mainly carried out on the basis of blowing and trapping, and substances which have influences on the food quality can migrate into the food in the process that the printed packaging paper is in direct or indirect contact with the food, so that the safety of the food product cannot be guaranteed only by the residual quantity detection.
Disclosure of Invention
In view of the above-mentioned drawbacks of the prior art, an object of the present invention is to provide a method for detecting the migration amount of volatile organic compounds in a paper packaging material into a dry simulant, which is used to solve the problem that the migration amount cannot be directly detected during the prior art.
To achieve the above objects and other related objects, the present invention is achieved by the following technical solutions.
The invention provides a method for detecting the migration amount of volatile organic compounds in a paper packaging material to a dry simulant, wherein a standard sample and a sample to be detected capture the volatile organic compounds by a purging and trapping method respectively, wherein the standard sample is a standard working solution formed by adding a certain amount of the dry simulant into a series of volatile organic compounds with different concentrations respectively; the volatile organic compound is selected from ethanol, isopropanol, n-propanol, ethyl acetate, 1-methoxy-2-propanol and n-propyl acetate;
the sample to be measured is an aqueous solution formed by adding the same amount of dry simulant into water after the migration treatment is carried out on the dry simulant by adopting a paper packaging material, wherein the volume of the added water is the same as the volume of the added volatile organic compounds when the standard sample is prepared;
the detection method comprises the following steps:
purging the standard sample to trap volatile organic compounds; then desorption and gas chromatography mass spectrometry are carried out to obtain corresponding response values;
establishing a standard curve according to the response value of the volatile organic compounds in the standard sample and the concentration of the volatile organic compounds in the standard sample;
purging and trapping volatile organic compounds in a sample to be detected; then desorption and gas chromatography mass spectrometry are carried out to obtain corresponding response values; and obtaining the concentration of the volatile organic compounds in the sample to be detected according to the response value of the volatile organic compounds in the sample to be detected and the standard curve, and taking the measured concentration as the migration volume of the volatile organic compounds in the sample to be detected.
The purging and trapping method is a dynamic headspace technique, which comprises the steps of purging volatile components in a sample by using flowing gas, adsorbing purged organic matters by using a trap, and then sending the sample into a gas chromatograph for analysis by thermal desorption.
According to the technical scheme, the standard sample or the sample to be detected can be added into the purging tube, the purging tube is placed in the purging and trapping sample injector after mixing, the purging tube is purged by the purging gas at room temperature after heating, and the purging tube enters the gas chromatography mass spectrum for analysis after trapping and desorption. Preferably, agitation and centrifugation means are also used to ensure adequate mixing during mixing.
According to the technical scheme of the invention, the oscillation is realized by adopting a vortex oscillator. Preferably, vortex oscillation is employed. More specifically, the oscillation rate is 500r/min-2000r/min, and the oscillation time is 2min-10 min. More specifically, the oscillation rate is 2000r/min, and the oscillation time is 5 min.
According to the technical scheme of the invention, the centrifugation speed is 4000r/min-5000r/min, and the centrifugation time is 5min-10 min. More specifically, the centrifugation rate is 5000r/min and the centrifugation time is 10 min.
According to the technical scheme of the invention, the concentration of the volatile organic compound aqueous solution of the standard working solution of the volatile organic compound in the standard sample is 0.01-12 mu g/mL by taking the mass of the volatile organic compound as a reference.
According to the technical scheme, the dry simulant is made of modified polyphenyl ether. Its chemical name can be written as Tenax.
According to the technical scheme of the invention, the volatile organic compounds comprise six of ethanol, isopropanol, n-propanol, ethyl acetate, 1-methoxy-2-propanol and n-propyl acetate, and the six organic compounds may exist in paper packaging materials and may migrate to contact materials.
According to the technical scheme, the method for carrying out migration treatment by adopting the paper packaging material comprises the step of placing the dry simulant and the paper packaging material into a closed container together and placing the closed container for more than 7 days at the temperature of 30-50 ℃. Specifically, the sheet may be left at 40 ℃ for 10 days. More preferably, the non-printed side of the paper wrapper is in contact with a dry simulant.
According to the technical scheme, the purging tube is made of brown glass, the matched screw cap is a silica gel spacer which comprises PTFE/silica gel spacers, and the volume of the purging tube is 30-40 mL.
More preferably, the material of the matched screw cap of the purging pipe is a low-loss PTFE/silica gel spacer.
More preferably, the purge tube volume is 40 mL.
Preferably, the dry simulant mass is between 0.5g and 5 g. More preferably, the dry simulant mass is 1 g.
Preferably, the volume of the standard working solution of volatile organic compounds is 5mL to 10mL when the mass of the dry simulant is 1 g. More preferably, the volume of the standard working solution of volatile organic compounds is 5 mL.
According to the technical scheme of the invention, the temperature of the base of the sample injector is set to be 40-80 ℃ during heating. The temperature can be adopted to heat the sample to be measured or the standard sample to 40-80 ℃; preferably 80 deg.c.
According to the technical scheme of the invention, the purging time is 5min-15min, and the purging flow is 20mL/min-40 mL/min. In a more specific embodiment, the purge time is 11min and the purge flow is 40 mL/min.
According to the technical scheme of the invention, the purge gas is helium. In particular to high-purity helium with the purity of 99.999 percent.
According to the technical scheme of the invention, the room temperature is 20-25 ℃.
According to the technical scheme of the invention, the temperature during desorption is 230-280 ℃, and the desorption time is 1-3 min. More specifically, the desorption temperature is 250 ℃, and the desorption time is 2 min.
According to the technical scheme of the invention, the response value of each volatile organic compound in the standard sample is used as the ordinate of the standard curve, and the concentration of the volatile organic compound is used as the abscissa of the standard curve.
As described above, the present invention provides a method for detecting the migration amount of volatile organic compounds in a paper packaging material into a dry simulant, which has the following beneficial effects:
1) the invention applies the blowing and trapping technology to the detection of the migration quantity of volatile organic compounds in the paper packaging material to the dry simulant for the first time.
2) The invention adopts the purging and trapping technology, obtains the migration volume information by directly heating, purging, trapping, desorbing and analyzing, and improves the detection sensitivity compared with a static headspace method.
3) The invention adopts the purging and trapping technology, obtains the migration amount information by directly heating, purging, trapping, desorbing and analyzing, does not need a complex extraction process, and improves the simplicity of the detection of the migration amount.
4) The invention applies the blowing and trapping technology to the detection of the migration amount of volatile organic compounds in the paper packaging material to the dry simulant, does not need to use an organic solvent, saves the detection cost and improves the environmental friendliness of the method.
5) The method is based on the blowing and trapping gas-mass combination technology to directly acquire the signal of the standard solution added with the dry simulant so as to establish the standard curve, and the portability of establishing the standard curve is improved.
Detailed Description
The embodiments of the present invention are described below with reference to specific embodiments, and other advantages and effects of the present invention will be easily understood by those skilled in the art from the disclosure of the present specification. The invention is capable of other and different embodiments and of being practiced or of being carried out in various ways, and its several details are capable of modification in various respects, all without departing from the spirit and scope of the present invention.
It is to be understood that the processing equipment or apparatus not specifically identified in the following examples is conventional in the art.
Furthermore, it is to be understood that one or more method steps mentioned in the present invention does not exclude that other method steps may also be present before or after the combined steps or that other method steps may also be inserted between these explicitly mentioned steps, unless otherwise indicated; it is also to be understood that a combined connection between one or more devices/apparatus as referred to in the present application does not exclude that further devices/apparatus may be present before or after the combined device/apparatus or that further devices/apparatus may be interposed between two devices/apparatus explicitly referred to, unless otherwise indicated. Moreover, unless otherwise indicated, the numbering of the various method steps is merely a convenient tool for identifying the various method steps, and is not intended to limit the order in which the method steps are arranged or the scope of the invention in which the invention may be practiced, and changes or modifications in the relative relationship may be made without substantially changing the technical content.
Example 1
1. Establishing a standard working curve
100mg of ethanol, 15mg of isopropanol, 15mg of n-propanol, 150mg of ethyl acetate, 500mg of 1-methoxy-2-propanol and 100mg of n-propyl acetate are respectively transferred into a 100mL volumetric flask, the volume is determined by water, a first-grade standard stock solution is prepared, and the stock solution is sealed and stored away from light under the condition of 0-4 ℃.
Respectively transferring 5mL of the primary standard stock solution into a 100mL volumetric flask, adding water to a constant volume, preparing a secondary standard stock solution, and storing in a sealed and light-proof manner at the temperature of 0-4 ℃.
Accurately transferring 4mL, 2mL, 1.5mL, 1mL, 0.5mL and 0.25mL of secondary standard stock solutions into a 100mL volumetric flask, and adding water to constant volume to obtain six-grade series standard working solutions.
Weighing 1g Tenax in six purging bottles respectively, adding 5mL series of standard working solutions respectively, oscillating for 5min on a vortex oscillator (2000r/min), centrifuging (5000r/min) for 10min, heating by a sample injector at 80 ℃, purging by high-purity helium (purity 99.999%) at room temperature, trapping, desorbing and then carrying out GC/MS analysis.
And (4) taking the concentration of the volatile organic compounds in the standard solution as an abscissa and taking the GC/MS response peak area as an ordinate to draw a standard curve. The detection limit and the quantitative limit are examined and are shown in table 1 in detail.
From table 1, it can be seen that: correlation coefficient R of standard curve of 6 solvents
2The correlation is better when the correlation is larger than 0.997; the detection limit is 0.0015 mu g/mL-0.1300 mu g/mL, which indicates that the method has higher sensitivity.
TABLE 1 Standard working curves, detection limits, quantification limits
2. Accuracy and precision of the method
The accuracy and precision of the method were examined by recovery rate test, 1g of dry simulant was added with 3 levels of standard solutions, low, medium and high, respectively, 3 samples were measured at each level, the content of volatile organic compounds was measured, and the recovery rate and precision of the method were calculated, and the results are shown in table 2. The recovery rate is the ratio of the transfer capacity test value to the transfer capacity theoretical value, and the average recovery rate is the average value of the recovery rates obtained by 3 times of tests; the precision refers to the relative standard deviation of the migration amount test value obtained by three tests, specifically the ratio of the standard deviation to the average value.
As can be seen from Table 2, the average recovery rate of 6 volatile organic compounds is between 87.83% and 139.13%, wherein the average recovery rate of other volatile organic compounds is within an error range of 16% except for n-propyl acetate, and considering that the air contains more n-propyl acetate due to more n-propyl acetate-containing materials used in the company test environment, the error of the n-propyl acetate formation is larger, and this interference data can be eliminated during accuracy evaluation, and the method in the application has better accuracy according to the average recovery rate values of other volatile organic compounds, and can be used as a method for evaluating the migration amount; the RSD for measuring the precision is between 0.33% and 11.55%, the precision error is within 15% according to the RSD value, and the method is good and suitable for evaluating the migration quantity.
TABLE 2 recovery, precision
3. Migration test of wrapping paper sample
Weighing 1g Tenax, uniformly spreading into a glass culture flask, and cutting to 0.25dm
2The wrapper sample was placed over Tenax (printed side up) and then sealed with a lid. The petri dish was placed in an oven and equilibrated at 40 ℃ for 10 days, taken out and cooled to room temperature.
Transferring the Tenax in the culture dish into a purging tube, adding 5mL of ultrapure water, performing vortex oscillation on a vortex oscillator at a speed of 2000r/min for 5min, and centrifuging at 5000r/min for 10 min; after heating at 80 ℃ by a sample injector, the sample was purged with a purge gas (purity 99.999%) at room temperature, and the gas was collected and desorbed, and then subjected to GC/MS analysis.
4. Actual sample detection
The method established in the text is adopted to detect the migration amount of 6 types of volatile organic compounds in part of the packaging paper, and the migration rate is researched, wherein the migration rate is the ratio of the migration amount to the residual amount, and the residual amount refers to the amount of the volatile organic compounds contained in the paper packaging material.
From the results, it can be seen that the mobility of ethanol is 0% to 3.08%; the mobility of the isopropanol is 2.69-4.40%; the mobility of the n-propanol is 2.94% -6.57%; the mobility of the ethyl acetate is 0 to 5.90 percent; the mobility of 1-methoxy-2-propanol was 0%; the mobility of the n-propyl acetate is 2.13% -12.23%.
Table 3: residual quantity, migration quantity and migration rate of volatile organic compounds in packaging paper
The residual amounts in table 3 refer to the content of volatile organic compounds contained in the paper materials used in the examples.
Example 2
1. Establishing a standard working curve
100mg of ethanol, 15mg of isopropanol, 15mg of n-propanol, 150mg of ethyl acetate, 500mg of 1-methoxy-2-propanol and 100mg of n-propyl acetate are transferred into a 100mL volumetric flask, the volume is determined by water, a first-grade standard stock solution is prepared, and the stock solution is sealed and stored away from light under the condition of 0-4 ℃.
And (3) transferring 5mL of the primary standard stock solution into a 100mL volumetric flask, adding water to a constant volume, preparing a secondary standard stock solution, and storing the secondary standard stock solution in a sealed and light-proof manner at the temperature of 0-4 ℃.
Accurately transferring 4mL, 2mL, 1.5mL, 1mL, 0.5mL and 0.25mL of secondary standard stock solutions into a 100mL volumetric flask, and diluting to constant volume with water to obtain six-level series standard working solutions.
Weighing 1g Tenax in six purging bottles respectively, adding 5mL series of standard working solutions respectively, oscillating for 5min on a vortex oscillator (2000r/min), centrifuging (5000r/min) for 10min, heating by a sample injector at 80 ℃, purging by high-purity helium (purity 99.999%) at room temperature, trapping, desorbing and then carrying out GC/MS analysis.
And (4) taking the concentration of the measured object in the standard solution as an abscissa and taking the GC/MS response peak area as an ordinate to draw a standard curve.
2. Migration experiment of sample of wrapping paper with barrier layer
Weighing 1g Tenax, uniformly spreading into a glass culture flask, and cutting to 0.25dm
2Barrier layer sample, placed over Tenax, and the wrapper sample (printed side up) was placed over the barrier layer and then sealed with a cap. The petri dish was placed in an oven and equilibrated at 40 ℃ for 10 days, taken out and cooled to room temperature.
Transferring the Tenax in the culture dish into a purging tube, adding 5mL of ultrapure water, performing vortex oscillation on a vortex oscillator at a speed of 2000r/min for 5min, and centrifuging at 5000r/min for 10 min; after heating at 80 ℃ by a sample injector, the sample was purged with a purge gas (purity 99.999%) at room temperature, and the gas was collected and desorbed, and then subjected to GC/MS analysis.
3. Actual sample detection
The migration amount of 6 volatile organic compounds in the packaging paper sample added with the barrier layer is detected by the method established in the text, and the migration rate value index is researched, so that the migration rate of ethanol in the packaging paper sample without the barrier layer is 0.59 percent; the mobility of isopropanol was 2.73%; the mobility of ethyl acetate was 0%; the mobility of n-propyl acetate was 7.82%. After the barrier layer is added, the ethanol mobility of the packaging paper sample is 0.38%; the mobility of isopropanol was 2.41%; the mobility of ethyl acetate was 0%; the mobility of n-propyl acetate was 7.35%. As can be seen from the data of sample 5, there was a certain reduction in migration after increasing the barrier layer.
Table 4: residual quantity, migration quantity and migration rate of volatile organic compounds in packaging paper
The foregoing embodiments are merely illustrative of the principles and utilities of the present invention and are not intended to limit the invention. Any person skilled in the art can modify or change the above-mentioned embodiments without departing from the spirit and scope of the present invention. Accordingly, it is intended that all equivalent modifications or changes which can be made by those skilled in the art without departing from the spirit and technical spirit of the present invention be covered by the claims of the present invention.
Claims (10)
1. A detection method for migration quantity of volatile organic compounds in a paper packaging material to a dry simulant is characterized in that a standard sample and a sample to be detected are used for trapping and testing the volatile organic compounds respectively through a purging and trapping method, wherein the standard sample is a standard working solution formed by adding a certain amount of the dry simulant to a series of volatile organic compounds with different concentrations respectively; the volatile organic compound is selected from ethanol, isopropanol, n-propanol, ethyl acetate, 1-methoxy-2-propanol and n-propyl acetate;
the sample to be measured is an aqueous solution formed by adding the same amount of dry simulant into water after the migration treatment is carried out on the dry simulant by adopting a paper packaging material, wherein the volume of the added water is the same as the volume of the added volatile organic compounds when the standard sample is prepared;
the detection method comprises the following steps:
purging the standard sample to trap volatile organic compounds; then desorption and gas chromatography mass spectrometry are carried out to obtain corresponding response values;
establishing a standard curve according to the response value of the volatile organic compounds in the standard sample and the concentration of the volatile organic compounds in the standard sample;
purging and trapping volatile organic compounds in a sample to be detected; then desorption and gas chromatography mass spectrometry are carried out to obtain corresponding response values;
and obtaining the concentration of the volatile organic compounds in the sample to be detected according to the response value of the volatile organic compounds in the sample to be detected and the standard curve, and taking the measured concentration as the migration volume of the volatile organic compounds in the sample to be detected.
2. The detection method according to claim 1, wherein the standard sample or the sample to be detected is added into a purge tube, after mixing, the purge tube is placed in a purge and trap sample injector, after heating, the purge tube is purged with purge gas at room temperature, and after trapping and desorption, the purge tube is subjected to gas chromatography mass spectrometry for analysis.
3. The method of claim 1, wherein the dry mimic is a modified polyphenylene ether material.
4. The detection method according to claim 1, wherein the migration treatment is performed by placing the dry simulant and the paper packaging material together in a closed container at 30-50 ℃ for 7 days or more.
5. The detection method according to claim 1, wherein the dry simulant mass is 0.5g to 5 g.
6. The detection method according to claim 1, wherein the volume of the standard working solution of volatile organic compounds is 5mL to 10mL when the mass of the dry simulant is 1 g.
7. The detection method according to claim 2, wherein the temperature of the injector base is set to 40 ℃ to 80 ℃ during heating.
8. The detection method according to claim 2, characterized by comprising one or more of the following features:
the purging time is 5min-15 min;
the purging flow is 20mL/min-40 mL/min;
the purge gas is helium.
9. The detection method according to claim 2, characterized by comprising one or both of the following features:
the temperature during desorption is 230-280 ℃;
the desorption time is 1min-3 min.
10. The detection method according to claim 1, wherein the standard working solution of volatile organic compounds in the standard sample is an aqueous solution of volatile organic compounds at a concentration of 0.01 μ g/mL to 11 μ g/mL based on the mass of volatile organic compounds.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201911058776.8A CN110780000A (en) | 2019-11-01 | 2019-11-01 | Method for detecting migration amount of volatile organic compounds in paper packaging material to dry simulant |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201911058776.8A CN110780000A (en) | 2019-11-01 | 2019-11-01 | Method for detecting migration amount of volatile organic compounds in paper packaging material to dry simulant |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN110780000A true CN110780000A (en) | 2020-02-11 |
Family
ID=69388607
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201911058776.8A Pending CN110780000A (en) | 2019-11-01 | 2019-11-01 | Method for detecting migration amount of volatile organic compounds in paper packaging material to dry simulant |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN110780000A (en) |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111624290A (en) * | 2020-05-11 | 2020-09-04 | 中国包装科研测试中心 | Method for determining VOCs in packaging material by purging and trapping-gas chromatography-mass spectrometry |
| CN112014505A (en) * | 2020-08-31 | 2020-12-01 | 广西大学 | Method for detecting content of methanol or ethanol in power transformer insulating paper |
| CN112858502A (en) * | 2021-01-06 | 2021-05-28 | 徐州市质量技术监督综合检验检测中心(徐州市标准化研究中心) | Method for detecting migration quantity of volatile organic compounds in food contact material and product in oil-based simulant |
| 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 |
| 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 |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102128906A (en) * | 2010-12-27 | 2011-07-20 | 中国烟草总公司郑州烟草研究院 | Method for detecting volatile organic compound in cigarette filter |
| CN104215732A (en) * | 2014-09-26 | 2014-12-17 | 云南中烟工业有限责任公司 | Method of taking Tenax as simulant to measure migration amount from paper and volatile and semi-volatile organic matter in paperboard by TD-GC/MS |
| CN104215719A (en) * | 2014-09-26 | 2014-12-17 | 云南中烟工业有限责任公司 | Purge and trap method for measuring migration volume of particular volatile and semi-volatile substances of paper and paperboards by using water as mimetic |
| CN105866267A (en) * | 2016-03-29 | 2016-08-17 | 福建中烟工业有限责任公司 | Method for extracting residual solvent in packaging material, method for detecting residual solvent, kit for detecting residual solvent, and use of kit |
-
2019
- 2019-11-01 CN CN201911058776.8A patent/CN110780000A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102128906A (en) * | 2010-12-27 | 2011-07-20 | 中国烟草总公司郑州烟草研究院 | Method for detecting volatile organic compound in cigarette filter |
| CN104215732A (en) * | 2014-09-26 | 2014-12-17 | 云南中烟工业有限责任公司 | Method of taking Tenax as simulant to measure migration amount from paper and volatile and semi-volatile organic matter in paperboard by TD-GC/MS |
| CN104215719A (en) * | 2014-09-26 | 2014-12-17 | 云南中烟工业有限责任公司 | Purge and trap method for measuring migration volume of particular volatile and semi-volatile substances of paper and paperboards by using water as mimetic |
| CN105866267A (en) * | 2016-03-29 | 2016-08-17 | 福建中烟工业有限责任公司 | Method for extracting residual solvent in packaging material, method for detecting residual solvent, kit for detecting residual solvent, and use of kit |
Non-Patent Citations (1)
| Title |
|---|
| 汪宣 等: "吹扫捕集气质联用法检测纸质包装材料中6种挥发牲有机物的迁移量", 《印刷质量与标准化》 * |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111624290A (en) * | 2020-05-11 | 2020-09-04 | 中国包装科研测试中心 | Method for determining VOCs in packaging material by purging and trapping-gas chromatography-mass spectrometry |
| CN112014505A (en) * | 2020-08-31 | 2020-12-01 | 广西大学 | Method for detecting content of methanol or ethanol in power transformer insulating paper |
| CN112014505B (en) * | 2020-08-31 | 2022-10-11 | 广西大学 | Method for detecting content of methanol or ethanol in power transformer insulating paper |
| CN112858502A (en) * | 2021-01-06 | 2021-05-28 | 徐州市质量技术监督综合检验检测中心(徐州市标准化研究中心) | Method for detecting migration quantity of volatile organic compounds in food contact material and product in oil-based simulant |
| 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 |
| 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 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN110780000A (en) | Method for detecting migration amount of volatile organic compounds in paper packaging material to dry simulant | |
| CN101876652B (en) | Method for measuring benzene and benzene series in printing ink | |
| CN109870526A (en) | A method of trimethylamine content in air is measured by Headspace-Gas Chromatography Analysis | |
| CN105738539A (en) | Method for determining content of trimethylamine in egg yolk through headspace gas chromatography | |
| Panavaitė et al. | Silicone glue coated stainless steel wire for solid phase microextraction | |
| CN113504333B (en) | Method for detecting organic matter migration amount in paper packaging material | |
| CN113341018B (en) | Method for measuring migration quantity of 10 volatile and semi-volatile compounds in packaging printing paper to MPPO | |
| CN105527353B (en) | A kind of method that utilization tracer headspace gas chromatography determines organic solvent solubility | |
| CN110658265A (en) | Method for simultaneously measuring contents of benzene, toluene, xylene and naphthalene in coal gas | |
| Li et al. | Solvent vapour monitoring in work space by solid phase micro extraction | |
| CN101592632B (en) | Method for measuring and analyzing content of acetone contained in power transformer oil | |
| WO2023065811A1 (en) | Method for measuring content of methanol in burst bead essential oil for cigarette | |
| CN110297053A (en) | A kind of food contact quick screening method of solvent residual amount in packaging material | |
| Yang et al. | An in‐needle solid‐phase microextraction device packed with etched steel wires for polycyclic aromatic hydrocarbons enrichment in water samples | |
| Li et al. | Solid-phase microextraction coupled to gas chromatography for the determination of 2, 3-dimethyl-2, 3-dinitrobutane as a marking agent for explosives | |
| WO2023087825A1 (en) | Method for measuring moisture content in cigarette burst bead | |
| CN111983062B (en) | Method for detecting trace DMAEA in air | |
| Chen et al. | The application research of solid‐phase extraction and headspace gas chromatography in the detection of methanol in transformer oil | |
| Hernández-Munoz et al. | Simple method for the selection of the appropriate food simulant for the evaluation of a specific food/packaging interaction | |
| CN108387649A (en) | Detection method that is a kind of while detecting a variety of pernicious gases in workplace | |
| Xie et al. | Method for improving accuracy in full evaporation headspace analysis | |
| CN108680659A (en) | The method for measuring volatile organic compounds in water using portable head space-gas chromatograph-mass spectrometer | |
| CN107727782B (en) | Method for determining effective content of AKD emulsion by ionic liquid-assisted headspace gas chromatography | |
| Xie et al. | A double sealing technique for increasing the precision of headspace-gas chromatographic analysis | |
| He et al. | Quantitative prediction of ionic liquid-gas partition coefficients for residual solvents by HS-GC |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20200211 |