CN103575848B - Method for determining migration quantity of volatile organic compounds in adhesive sticker for food label in water-based food simulating object - Google Patents
Method for determining migration quantity of volatile organic compounds in adhesive sticker for food label in water-based food simulating object Download PDFInfo
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- 235000013305 food Nutrition 0.000 title claims abstract description 61
- 239000000853 adhesive Substances 0.000 title claims abstract description 43
- 230000001070 adhesive effect Effects 0.000 title claims abstract description 42
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 title claims abstract description 23
- 238000013508 migration Methods 0.000 title claims abstract description 14
- 230000005012 migration Effects 0.000 title claims abstract description 14
- 238000000034 method Methods 0.000 title abstract description 11
- 239000012855 volatile organic compound Substances 0.000 title abstract 6
- CRSBERNSMYQZNG-UHFFFAOYSA-N 1-dodecene Chemical compound CCCCCCCCCCC=C CRSBERNSMYQZNG-UHFFFAOYSA-N 0.000 claims abstract description 14
- QPUYECUOLPXSFR-UHFFFAOYSA-N 1-methylnaphthalene Chemical compound C1=CC=C2C(C)=CC=CC2=C1 QPUYECUOLPXSFR-UHFFFAOYSA-N 0.000 claims abstract description 14
- JRZJOMJEPLMPRA-UHFFFAOYSA-N 1-nonene Chemical compound CCCCCCCC=C JRZJOMJEPLMPRA-UHFFFAOYSA-N 0.000 claims abstract description 14
- UFWIBTONFRDIAS-UHFFFAOYSA-N Naphthalene Chemical compound C1=CC=CC2=CC=CC=C21 UFWIBTONFRDIAS-UHFFFAOYSA-N 0.000 claims abstract description 14
- HFJRKMMYBMWEAD-UHFFFAOYSA-N dodecanal Chemical compound CCCCCCCCCCCC=O HFJRKMMYBMWEAD-UHFFFAOYSA-N 0.000 claims abstract description 14
- 238000010926 purge Methods 0.000 claims abstract description 14
- SQNZJJAZBFDUTD-UHFFFAOYSA-N durene Chemical compound CC1=CC(C)=C(C)C=C1C SQNZJJAZBFDUTD-UHFFFAOYSA-N 0.000 claims abstract description 12
- KJIOQYGWTQBHNH-UHFFFAOYSA-N undecanol Chemical compound CCCCCCCCCCCO KJIOQYGWTQBHNH-UHFFFAOYSA-N 0.000 claims abstract description 8
- DSSYKIVIOFKYAU-XCBNKYQSSA-N (R)-camphor Chemical compound C1C[C@@]2(C)C(=O)C[C@@H]1C2(C)C DSSYKIVIOFKYAU-XCBNKYQSSA-N 0.000 claims abstract description 7
- GOXQRTZXKQZDDN-UHFFFAOYSA-N 2-Ethylhexyl acrylate Chemical compound CCCCC(CC)COC(=O)C=C GOXQRTZXKQZDDN-UHFFFAOYSA-N 0.000 claims abstract description 7
- YIWUKEYIRIRTPP-UHFFFAOYSA-N 2-ethylhexan-1-ol Chemical compound CCCCC(CC)CO YIWUKEYIRIRTPP-UHFFFAOYSA-N 0.000 claims abstract description 7
- 241000723346 Cinnamomum camphora Species 0.000 claims abstract description 7
- 229960000846 camphor Drugs 0.000 claims abstract description 7
- 229930008380 camphor Natural products 0.000 claims abstract description 7
- 229940069096 dodecene Drugs 0.000 claims abstract description 7
- 229940075566 naphthalene Drugs 0.000 claims abstract description 5
- 238000010812 external standard method Methods 0.000 claims abstract description 4
- 238000005070 sampling Methods 0.000 claims abstract description 4
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 30
- 239000000243 solution Substances 0.000 claims description 27
- 238000002372 labelling Methods 0.000 claims description 14
- 238000002360 preparation method Methods 0.000 claims description 12
- 239000005416 organic matter Substances 0.000 claims description 7
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 6
- 238000003556 assay Methods 0.000 claims description 6
- 239000012159 carrier gas Substances 0.000 claims description 6
- 238000003795 desorption Methods 0.000 claims description 6
- 239000012086 standard solution Substances 0.000 claims description 6
- 238000004817 gas chromatography Methods 0.000 claims description 4
- 238000002347 injection Methods 0.000 claims description 4
- 239000007924 injection Substances 0.000 claims description 4
- 238000000642 dynamic headspace extraction Methods 0.000 claims description 3
- 238000001819 mass spectrum Methods 0.000 claims description 3
- 229910052757 nitrogen Inorganic materials 0.000 claims description 3
- 230000002000 scavenging effect Effects 0.000 claims description 3
- 238000007789 sealing Methods 0.000 claims description 3
- 238000002791 soaking Methods 0.000 claims description 3
- 229910021642 ultra pure water Inorganic materials 0.000 claims description 3
- 239000012498 ultrapure water Substances 0.000 claims description 3
- 238000004949 mass spectrometry Methods 0.000 abstract description 4
- 238000001514 detection method Methods 0.000 abstract description 3
- 230000035945 sensitivity Effects 0.000 abstract description 2
- 238000012360 testing method Methods 0.000 abstract 2
- 238000004519 manufacturing process Methods 0.000 abstract 1
- BGEHHAVMRVXCGR-UHFFFAOYSA-N methylundecylketone Natural products CCCCCCCCCCCCC=O BGEHHAVMRVXCGR-UHFFFAOYSA-N 0.000 abstract 1
- 238000011002 quantification Methods 0.000 abstract 1
- NIXOWILDQLNWCW-UHFFFAOYSA-N acrylic acid group Chemical group C(C=C)(=O)O NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 description 3
- 239000007767 bonding agent Substances 0.000 description 3
- 239000004831 Hot glue Substances 0.000 description 2
- 238000004458 analytical method Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- -1 2-Ethylhexyl Alcohols Chemical class 0.000 description 1
- 241000143060 Americamysis bahia Species 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000009472 formulation Methods 0.000 description 1
- 235000012055 fruits and vegetables Nutrition 0.000 description 1
- 230000008676 import Effects 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 235000013372 meat Nutrition 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 150000002894 organic compounds Chemical class 0.000 description 1
- 238000012856 packing Methods 0.000 description 1
- 238000010422 painting Methods 0.000 description 1
- 239000003755 preservative agent Substances 0.000 description 1
- 230000002335 preservative effect Effects 0.000 description 1
- 238000004445 quantitative analysis Methods 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 238000010561 standard procedure Methods 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
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- Other Investigation Or Analysis Of Materials By Electrical Means (AREA)
Abstract
The invention discloses a method for determining the migration quantity of volatile organic compounds in an adhesive sticker for a food label in a water-based food simulating object. The method comprises the following steps: performing a direct or indirect migration test on the adhesive sticker for the food label through a water-based food simulating solution; sampling the water-based food simulating solution through purging and trapping; separating 10 volatile organic compounds through HP-5ms or chromatographic columns with similar properties; performing detection through a mass spectrometry detector; performing quantification through an external standard method, wherein the 10 volatile organic compounds include nonene, 2-ethylhexanol, 1,2,4,5-tetramethylbenzene, camphor, 1-dodecene, naphthalene, 2-ethylhexyl acrylate, 1-methylnaphthalene, 1-undecanol and dodecyl aldehyde. The method is accurate in test, easy to operate, high in efficiency, quick, high in sensitivity and high in practicality, is applicable to qualitative and quantitative determination on the volatile organic compounds in the adhesive sticker for the food label through a manufacturing enterprise of the adhesive sticker for the food label and relevant government supervision departments, and can be used for avoiding harm to the physical health of a consumer caused by over-large migration quantity of the volatile organic compounds.
Description
Technical field
The present invention relates to the assay method of volatile organic matter migration amount in water base food analogies in adhesive sticker for a kind of food labelling.
Background technology
Adhesive label is also self-adhesive label, posting in time, Sticky Note, impact paper etc., and the basic structure of adhesive label from top to bottom order is coated with and is formed by surface-coated, surfacing, linging, bonding agent, painting silicon layer, base stock and the back of the body.Wherein directly contact with food or the part of indirect contact is bonding agent, its principal ingredient is rubber-based, elastic body or acrylic adhesives.
Adhesive label is used as food labelling and is seen everywhere, and particularly in large supermarket, no matter is fishes and shrimps, fresh meat, or cold dish, fruits and vegetables, and the label being attached on transparent packing bag or preservative film is the unique channel of checkout.Adhesive sticker food labelling is owing to directly contacting or indirect contact with food, its security and consumer health are closely bound up, yet the use for adhesive sticker food labelling bonding agent, at present all there is no relevant rules both at home and abroad, to various types of adhesive sticker food labelling, venture analysis is blank substantially.Do not have at present quantitative method to assess harmful volatile organic matter in adhesive label and move to the especially content in aqueous food of food.
Summary of the invention
The object of the present invention is to provide the assay method of volatile organic matter migration amount in water base food analogies in adhesive sticker for a kind of food labelling, it can measure food labelling rapidly and accurately with adhesive sticker directly or indirectly and during Food Contact, move to 10 kinds of volatile organic matters (nonene, 2-Ethylhexyl Alcohols, 1 in water base food analogies, 2,4,5-tetramethylbenzene, camphor, 1-dodecene, naphthalene, 2-ethylhexyl acrylate, 1-methylnaphthalene, 1-undecyl alcohol and lauric aldehyde) content.For the venture analysis of the food adhesive label method that provides the foundation, for the formulation of relevant hygienic standard and detection method provides scientific basis, import and export food label is implemented to risk class management with adhesive sticker and there is important directive significance.
The present invention is achieved in that the assay method of volatile organic matter migration amount in water base food analogies in adhesive sticker for described food labelling, and it comprises the following steps:
1) standard reserving solution preparation: take nonene, 2-Ethylhexyl Alcohol, 1,2,4,5-tetramethylbenzene, camphor, 1-dodecene, naphthalene, 2-ethylhexyl acrylate, 1-methylnaphthalene, 1-undecyl alcohol, each 0.1g of lauric aldehyde standard items, be placed in 10mL volumetric flask, with ethanol, be settled to scale;
2) standard solution preparation: above-mentioned standard reserving solution is diluted to the standard operation solution series of applicable concentration on demand with ultrapure water;
3) sample preparation that adhesive sticker directly contacts with food: 0.05 g adhesive sticker is evenly coated on the microslide of 7.5 cm * 2.5 cm, the microslide after applying is placed in to beaker, food simulated solution adds 2 mL with every square centimeter of sample and is added to beaker;
4) sample preparation of adhesive sticker and food indirect contact: 0.05 g adhesive sticker is evenly coated on the microslide of 7.5 cm * 2.5 cm, microslide after applying is affixed on to food container outside surface, in container, with every square centimeter of adhesive sticker sample, add 2 mL food simulated solutions, sealing;
5) soaking conditions: using respectively water, 10% ethanol, 20% ethanol as food simulated solution, soak 4 hours at 95 ℃;
6) purge and trap parameter is set: purge carrier gas: nitrogen; Purge temperature: 20 ℃, purge flow rate: 40 mL/min, purge time: 11 min; Desorption temperature: 250 ℃, desorption time: 2 min; Stoving temperature: 280 ℃, cure the time: 5 min; Sample bottle: 40 mL, scavenging duct: 10 mL, sample quantitatively encircles: 5 mL, auto injection;
7) gas chromatography mass spectrometer parameter is set: chromatographic column: HP-5ms 30 mm * 2.5 * 10, m * 0.25
-4the similar analytical column of mm capillary column or performance; Temperature programme: 40 ℃ of initial temperatures, keep 3 min, 15 ℃/min rises to 250 ℃, keeps 10 min; Injector temperature: 250 ℃; Mass spectrometer interface temperature: 280 ℃; Ion source temperature: 230 ℃; Quadrupole rod temperature: 150 ℃; Carrier gas: He, purity >99.999 %, 1.0 mL/min constant currents; Sample size: 1 * 10
-3mL; Input mode: split sampling, split ratio 5:1; Ionization mode: EI; Scanning of the mass spectrum mode: full scan (SCAN), for 10% ethanol, 20% ethanol simulated solution sample, sweep limit is 50-500 m/z, for water simulated solution sample, sweep limit is 30-500 m/z;
8) standard working curve is drawn: by step 6), 7) given instrument parameter is to step 2) the standard solution series that obtains measures, and take concentration as horizontal ordinate, chromatographic peak area is ordinate, drawing standard working curve;
9) the water base food simulated solution of the sample that sample determination: by step 6), 7) given instrument parameter obtains step 5) is measured, the standard working curve obtaining according to step 8), and external standard method is quantitative.
10) range of linearity of method and quantitative limit index are in Table 1.
Table 1 range of linearity and quantitative limit
Beneficial effect of the present invention is: it has set up the purge and trap-gaschromatographic mass spectrometry determination method of food labelling by 10 kinds of organic compounds migration amount in water base food analogies in adhesive sticker, overcome the shortcoming that gas chromatography cannot direct aqueous injection, greatly improved on the other hand detection sensitivity.Method highly sensitive, precision is good, can meet the requirement of real work.
Accompanying drawing explanation
Fig. 1 is 10 kinds of common organic gaschromatographic mass spectrometry figure in adhesive sticker for food labelling.
In figure: 1, nonene; 2,2-Ethylhexyl Alcohol; 3,1,2,4,5-tetramethylbenzene; 4, camphor; 5,1-dodecene; 6, naphthalene; 7,2-ethylhexyl acrylate; 8,1-methylnaphthalene; 9,1-undecyl alcohol; 10, lauric aldehyde.
Embodiment
The assay method of volatile organic matter migration amount in water base food analogies in adhesive sticker for food labelling of the present invention, it comprises the following steps:
1) standard reserving solution preparation: take nonene, 2-Ethylhexyl Alcohol, 1,2,4,5-tetramethylbenzene, camphor, 1-dodecene, naphthalene, 2-ethylhexyl acrylate, 1-methylnaphthalene, 1-undecyl alcohol, each 0.1g of lauric aldehyde standard items, be placed in 10mL volumetric flask, with ethanol, be settled to scale;
2) standard solution preparation: above-mentioned standard reserving solution is diluted to the standard operation solution series of applicable concentration on demand with ultrapure water;
3) sample preparation that adhesive sticker directly contacts with food: 0.05 g adhesive sticker is evenly coated on the microslide of 7.5 cm * 2.5 cm, the microslide after applying is placed in to beaker, food simulated solution adds 2 mL with every square centimeter of sample and is added to beaker;
4) sample preparation of adhesive sticker and food indirect contact: 0.05 g adhesive sticker is evenly coated on the microslide of 7.5 cm * 2.5 cm, microslide after applying is affixed on to food container outside surface, in container, with every square centimeter of adhesive sticker sample, add 2 mL food simulated solutions, sealing;
5) soaking conditions: using respectively water, 10% ethanol, 20% ethanol as food simulated solution, soak 4 hours at 95 ℃;
6) purge and trap parameter is set: purge carrier gas: nitrogen; Purge temperature: 20 ℃, purge flow rate: 40 mL/min, purge time: 11 min; Desorption temperature: 250 ℃, desorption time: 2 min; Stoving temperature: 280 ℃, cure the time: 5 min; Sample bottle: 40 mL, scavenging duct: 10 mL, sample quantitatively encircles: 5 mL, auto injection;
7) gas chromatography mass spectrometer parameter is set: chromatographic column: HP-5ms 30 mm * 2.5 * 10, m * 0.25
-4the similar analytical column of mm capillary column or performance; Temperature programme: 40 ℃ of initial temperatures, keep 3 min, 15 ℃/min rises to 250 ℃, keeps 10 min; Injector temperature: 250 ℃; Mass spectrometer interface temperature: 280 ℃; Ion source temperature: 230 ℃; Quadrupole rod temperature: 150 ℃; Carrier gas: He, purity >99.999 %, 1.0 mL/min constant currents; Sample size: 1 * 10
-3mL; Input mode: split sampling, split ratio 5:1; Ionization mode: EI; Scanning of the mass spectrum mode: full scan (SCAN), for 10% ethanol, 20% ethanol simulated solution sample, sweep limit is 50-500 m/z, for water simulated solution sample, sweep limit is 30-500 m/z;
8) standard working curve is drawn: by step 6), 7) given instrument parameter is to step 2) the standard solution series that obtains measures, and take concentration as horizontal ordinate, chromatographic peak area is ordinate, drawing standard working curve;
9) the water base food simulated solution of the sample that sample determination: by step 6), 7) given instrument parameter obtains step 5) is measured, the standard working curve obtaining according to step 8), and external standard method is quantitative.
10) range of linearity of method and quantitative limit index are in Table 1.
Table 1 range of linearity and quantitative limit
Fig. 1 is 10 kinds of common organic gaschromatographic mass spectrometry figure in adhesive sticker for food labelling.
In figure: 1, nonene; 2,2-Ethylhexyl Alcohol; 3,1,2,4,5-tetramethylbenzene; 4, camphor; 5,1-dodecene; 6, naphthalene; 7,2-ethylhexyl acrylate; 8,1-methylnaphthalene; 9,1-undecyl alcohol; 10, lauric aldehyde.
Embodiment mono-
While adopting said method to measure 3 kinds of acrylic type adhesive stickers (1#～3#) directly to contact with water base food analogies with a kind of hot melt adhesive (4#), the migration amount of each material, the results are shown in table 2.
Table 2 Direct Transfer experimental result unit: ng/mL
Note: nd-not detected.
Embodiment bis-
While adopting said method to measure 3 kinds of acrylic type adhesive stickers (1#～3#) and a kind of hot melt adhesive (4#) to insure film and PE freshness protection package and water base food analogies indirect contact by PE, the migration amount of each material, the results are shown in table 3.
Table 3 is migration experimental result unit: ng/mL indirectly
Note: nd-not detected.
Claims (1)
1. the assay method of volatile organic matter migration amount in water base food analogies in adhesive sticker for food labelling, it comprises the following steps:
1) standard reserving solution preparation: take nonene, 2-Ethylhexyl Alcohol, 1,2,4,5-tetramethylbenzene, camphor, 1-dodecene, naphthalene, 2-ethylhexyl acrylate, 1-methylnaphthalene, 1-undecyl alcohol, each 0.1g of lauric aldehyde standard items, be placed in 10mL volumetric flask, with ethanol, be settled to scale;
2) standard solution preparation: above-mentioned standard reserving solution is diluted to the standard operation solution series of applicable concentration on demand with ultrapure water;
3) sample preparation that adhesive sticker directly contacts with food: 0.05 g adhesive sticker is evenly coated on the microslide of 7.5 cm * 2.5 cm, the microslide after applying is placed in to beaker, food simulated solution adds 2 mL with every square centimeter of sample and is added to beaker;
4) sample preparation of adhesive sticker and food indirect contact: 0.05 g adhesive sticker is evenly coated on the microslide of 7.5 cm * 2.5 cm, microslide after applying is affixed on to food container outside surface, in container, with every square centimeter of adhesive sticker sample, add 2 mL food simulated solutions, sealing;
5) soaking conditions: using respectively water, 10% ethanol, 20% ethanol as food simulated solution, soak 4 hours at 95 ℃;
6) purge and trap parameter is set: purge carrier gas: nitrogen; Purge temperature: 20 ℃, purge flow rate: 40 mL/min, purge time: 11 min; Desorption temperature: 250 ℃, desorption time: 2 min; Stoving temperature: 280 ℃, cure the time: 5 min; Sample bottle: 40 mL, scavenging duct: 10 mL, sample quantitatively encircles: 5 mL, auto injection;
7) gas chromatography mass spectrometer parameter is set: chromatographic column: HP-5ms 30 mm * 2.5 * 10, m * 0.25
-4the similar analytical column of mm capillary column or performance; Temperature programme: 40 ℃ of initial temperatures, keep 3 min, 15 ℃/min rises to 250 ℃, keeps 10 min; Injector temperature: 250 ℃; Mass spectrometer interface temperature: 280 ℃; Ion source temperature: 230 ℃; Quadrupole rod temperature: 150 ℃; Carrier gas: He, purity >99.999 %, 1.0 mL/min constant currents; Sample size: 1 * 10
-3mL; Input mode: split sampling, split ratio 5:1; Ionization mode: EI; Scanning of the mass spectrum mode: full scan, for 10% ethanol, 20% ethanol simulated solution sample, sweep limit is 50-500 m/z, for water simulated solution sample, sweep limit is 30-500 m/z;
8) standard working curve is drawn: by step 6), 7) given instrument parameter is to step 2) the standard solution series that obtains measures, and take concentration as horizontal ordinate, chromatographic peak area is ordinate, drawing standard working curve;
9) the water base food simulated solution of the sample that sample determination: by step 6), 7) given instrument parameter obtains step 5) is measured, the standard working curve obtaining according to step 8), and external standard method is quantitative.
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| US20190316365A1 (en) * | 2018-04-12 | 2019-10-17 | Milliken & Company | Installation of Floorcovering Article on Chemically Abated Flooring Surface and Composite Article |
| CN108872421B (en) * | 2018-05-21 | 2021-08-31 | 珠海天祥粤澳质量技术服务有限公司 | Method for detecting migration amount of acrylic acid in food packaging material |
| CN109900780A (en) * | 2019-04-02 | 2019-06-18 | 厦门历思科技服务有限公司 | The online pretreating device of hair sample sample introduction |
| CN110031457A (en) * | 2019-04-15 | 2019-07-19 | 深圳安吉尔饮水产业集团有限公司 | The measuring method of ethyl alcohol the amount of migration in a kind of food contact material |
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