CN103575848A - 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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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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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105092764A (en) * | 2015-09-14 | 2015-11-25 | 浙江工业大学 | Method for detecting migration quantity of methacrylic acid in food plastic packaging material by using online derivatization-gas chromatography |
| CN108872421A (en) * | 2018-05-21 | 2018-11-23 | 深圳天祥质量技术服务有限公司 | The detection method of the specific transfer 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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| JPS5687428A (en) * | 1979-12-18 | 1981-07-16 | Kishimoto Akira | Oxygen absorbing agent for closely sealed package |
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| JPS5687428A (en) * | 1979-12-18 | 1981-07-16 | Kishimoto Akira | Oxygen absorbing agent for closely sealed package |
| EP1550872A2 (en) * | 2004-01-05 | 2005-07-06 | Bio-Med Photonics Co. Ltd. | Lateral flow quantitative assay method and strip, laser-induced epifluorescence detection device and small scanner therefor |
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| CRISTINA NERIN等: "Determination of partition and diffusion coefficients of components of two rubber adhesives in different multilayer materials", 《INTERNATIONAL JOURNAL OF ADHESION & ADHESIVES》 * |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105092764A (en) * | 2015-09-14 | 2015-11-25 | 浙江工业大学 | Method for detecting migration quantity of methacrylic acid in food plastic packaging material by using online derivatization-gas chromatography |
| CN108872421A (en) * | 2018-05-21 | 2018-11-23 | 深圳天祥质量技术服务有限公司 | The detection method of the specific transfer 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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