CN114295742A - Method for testing transfer amounts of chloropropanol and fatty acid ester in packaging material - Google Patents
Method for testing transfer amounts of chloropropanol and fatty acid ester in packaging material Download PDFInfo
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- CN114295742A CN114295742A CN202111551893.5A CN202111551893A CN114295742A CN 114295742 A CN114295742 A CN 114295742A CN 202111551893 A CN202111551893 A CN 202111551893A CN 114295742 A CN114295742 A CN 114295742A
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Abstract
The invention relates to a method for testing the migration volume of chloropropanol and fatty acid ester in a packaging material, which fills up the blank of the industry, and the current food packaging field is not related to any related detection of chloropropanol, can increase the existing detection items, reduce the harm caused by unsupervised chloropropanol, and is beneficial to promoting the establishment of the industry standard; the detection project is chloropropanol multicomponent detection, in the field of food detection, only 3-MCPD and 2-MCPD have supervision requirements, the detection method not only detects the two, but also detects other chloropropanol fatty acid esters, researches on harm of chloropropanol related products to human bodies are increased, and the detection method can be enriched.
Description
Technical Field
The invention belongs to the technical field of packaging material testing, and particularly relates to a method for testing the migration volume of chloropropanol and fatty acid ester in a packaging material.
Background
The chloropropanol is a compound formed by substituting hydroxyl on a glycerol structure by a chlorine atom, and mainly comprises the following components: 3-chloro-1, 2-propanediol (3-MCPD), 2-chloro-1, 3-propanediol (2-MCPD), 1, 3-dichloro-2-propanol (1, 3-DCP) and 2, 3-dichloro-1-propanol (2, 3-DCP) have acute and chronic toxic effects, are easy to cause tumors of some experimental animals to cause damage to kidneys and reproductive systems, and are internationally recognized food pollutants.
The epichlorohydrin is an important organic compound of an organic synthetic raw material and an intermediate, and can be used as a common raw material for manufacturing products such as various adhesives, medicines, pesticides, plasticizers, ion exchange resins and the like. Can also be used as a solvent for adhesives, coatings, paints, rubbers, resins, cellulose esters, cellulose ethers and the like. The packaging material containing epichlorohydrin is easily decomposed into chloropropanol when meeting water, fruit juice, soup and other liquids, and migrates into food to cause pollution.
In the past, the monitoring of the chloropropanol content in food is mainly used for measuring the chloropropanol pollution generated in the process of processing and storing the food, but the detection of the chloropropanol pollution in food contact materials has not attracted enough attention.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provide a method for testing the migration amount of chloropropanol and fatty acid ester in a packaging material.
The technical problem to be solved by the invention is realized by the following technical scheme:
a method for testing the migration volume of chloropropanol and fatty acid ester in a packaging material is characterized by comprising the following steps: the testing method comprises the following steps:
1) preparing chloropropanol standard working solution (1 mg/L): weighing a certain amount of 3-MCPD, 2MCPD, 1, 3DCP and 2, 3-DCP, placing in a 100mL volumetric flask, adding n-hexane for dilution to scale, and mixing uniformly for later use;
2) preparing a deuterated chloropropanol standard working solution (10 mg/L): weighing a certain amount of D5Putting 3-MCPD, 2-MCPD, 1, 3-DCP and 2, 3-DCP in a l00mL volumetric flask, diluting to scale with n-hexane, and mixing for later use;
3) migration: taking a packaging material to be detected as a sample, and controlling the volume ratio of the surface area of the sample to the volume of the food simulation liquid to be 60cm2Soaking at a ratio of 100mL and preparing a migration liquid;
4) purifying: taking 10mL of migration liquid, adding an internal standard, mixing, adding the migration liquid into a diatomite solid-phase extraction column, standing for 10min, leaching with 20mL of n-hexane, discarding an effluent liquid, eluting with 30mL of ethyl acetate, collecting an eluent, blowing nitrogen to concentrate until the eluent is completely dried, dissolving residues with 2mL of n-hexane, transferring the dissolved residues into an l0mL glass tube with a plug, adding 5mL of anhydrous sodium sulfate, uniformly mixing, and dehydrating to form a purified liquid;
5) derivatization: adding 50 mu L of heptafluorobutyrylimidazole into the purified solution, carrying out vortex mixing for 30s, carrying out heat preservation at 70 ℃ for 120min, taking out, cooling to room temperature, adding 5mL of NaCl solution with the mass fraction of 20%, carrying out vortex mixing for 1min, and standing for layering; transferring the n-hexane phase, adding about 0.5g of anhydrous sodium sulfate for drying, and filtering by using a 0.22 mu m filter membrane to a sample injection vial to serve as a sample solution to be detected;
6) gas chromatography-mass spectrometry: adding the sample solution to be detected in the sample injection vial into a gas chromatography-mass spectrometer for gas chromatography-mass spectrometry;
7) and (3) qualitative confirmation: chromatographic peaks of the sample to-be-detected liquid and the known standard working solution appear at the same retention time, and the target analyte can be qualitatively confirmed at the moment;
8) quantitative analysis: and taking the concentration of each standard substance as an abscissa and the ratio of the response value of each quantitative chromatogram to the corresponding response value of the internal standard as an ordinate, making a linear regression equation of the standard curve, and comparing and quantifying the ratio of the response value of the sample to the response value of the corresponding internal standard with the standard curve.
Moreover, the chromatographic conditions of the gas chromatography-mass spectrometer are as follows:
a chromatographic column: HP-5MS, column length 30m, internal diameter 0.25m, film thickness 0.25 m);
sample injection and carrier gas: helium gas;
flow rate: 2 mL/min;
sample inlet temperature: 220 ℃;
sample introduction amount: 1L, no shunt sampling;
the solvent delay time is 6 min;
temperature programming: maintaining at 50 deg.C for 1min, heating to 270 deg.C at 10 deg.C/min, and maintaining for 5 min;
the mass spectrum conditions of the gas chromatography-mass spectrometer are as follows:
ion source temperature: 230 ℃;
temperature of the quadrupole rods: 150 ℃;
an ionization mode: EI;
ionization energy: 70 eV;
mass scan range: 50-450 amu;
the measurement method comprises the following steps: SIM scanning;
furthermore, the temperature and time of the soaking solution and soaking condition transferred in the step 3) are selected according to GB31604.1-2015 and GB 5009.156-2016.
The invention has the advantages and beneficial effects that:
1. the method for testing the migration volume of the chloropropanol and the fatty acid ester in the packaging material makes up for the blank of the industry, does not relate to any relevant detection of the chloropropanol in the field of food packaging at present, can increase the existing detection items, reduces the harm caused by unsupervised chloropropanol, and is beneficial to promoting the establishment of the industry standard.
2. According to the method for testing the migration volume of chloropropanol and fatty acid ester in the packaging material, a test item is chloropropanol multicomponent detection, in the field of food detection, only 3-MCPD and 2-MCPD have supervision requirements, the method not only detects the two, but also detects other chloropropanol fatty acid ester, the research on the harm of chloropropanol related products to human bodies is increased, and the detection method can be enriched.
Drawings
FIG. 1 is a total ion flow diagram of a chloropropanol multicomponent derivative of the present invention.
Description of the reference numerals
1--D5-3-MCPD derivatives; 2-3-MCPD derivatives; 3- -D5-2-MCPD derivatives; 4-2-MCPD derivatives; 5-D5-1, 3-DCP derivatives; 6-1, 3-DCP derivatives; 7- -D52, 3-DCP derivatives 8- -2, 3-DCP derivatives.
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 testing the migration volume of chloropropanol and fatty acid ester in a packaging material is characterized by comprising the following steps: the testing method comprises the following steps:
1) preparing chloropropanol standard working solution (1 mg/L): weighing a certain amount of 3-MCPD, 2MCPD, 1, 3DCP and 2, 3-DCP, placing in a 100mL volumetric flask, adding n-hexane for dilution to scale, and mixing uniformly for later use;
2) preparing a deuterated chloropropanol standard working solution (10 mg/L): weighing a certain amount of D5Putting 3-MCPD, 2-MCPD, 1, 3-DCP and 2, 3-DCP in a l00mL volumetric flask, diluting to scale with n-hexane, and mixing for later use;
3) migration: taking a packaging material to be detected as a sample, and controlling the volume ratio of the surface area of the sample to the volume of the food simulation liquid to be 60cm2Soaking at a ratio of 100mL and preparing a migration liquid, wherein the selection of the temperature and time of the soaking liquid and the soaking condition refers to GB31604.1-2015 and GB 5009.156-2016;
4) purifying: taking 10mL of migration liquid, adding an internal standard, mixing, adding the migration liquid into a diatomite solid-phase extraction column, standing for 10min, leaching with 20mL of n-hexane, discarding an effluent liquid, eluting with 30mL of ethyl acetate, collecting an eluent, blowing nitrogen to concentrate until the eluent is completely dried, dissolving residues with 2mL of n-hexane, transferring the dissolved residues into an l0mL glass tube with a plug, adding 5mL of anhydrous sodium sulfate, uniformly mixing, and dehydrating to form a purified liquid;
5) derivatization: adding 50 mu L of heptafluorobutyrylimidazole into the purified solution, carrying out vortex mixing for 30s, carrying out heat preservation at 70 ℃ for 120min, taking out, cooling to room temperature, adding 5mL of NaCl solution with the mass fraction of 20%, carrying out vortex mixing for 1min, and standing for layering; transferring the n-hexane phase, adding about 0.5g of anhydrous sodium sulfate for drying, and filtering by using a 0.22 mu m filter membrane to a sample injection vial to serve as a sample solution to be detected;
6) gas chromatography-mass spectrometry: adding the sample solution to be detected in the sample injection vial into a gas chromatography-mass spectrometer for gas chromatography-mass spectrometry;
7) and (3) qualitative confirmation: chromatographic peaks of the sample to-be-detected liquid and the known standard working solution appear at the same retention time, and the target analyte can be qualitatively confirmed at the moment;
8) quantitative analysis: and taking the concentration of each standard substance as an abscissa and the ratio of the response value of each quantitative chromatogram to the corresponding response value of the internal standard as an ordinate, making a linear regression equation of the standard curve, and comparing and quantifying the ratio of the response value of the sample to the response value of the corresponding internal standard with the standard curve.
The chromatographic conditions of the gas chromatography-mass spectrometer were:
a chromatographic column: HP-5MS, column length 30m, internal diameter 0.25m, film thickness 0.25 m);
sample injection and carrier gas: helium gas;
flow rate: 2 mL/min;
sample inlet temperature: 220 ℃;
sample introduction amount: 1L, no shunt sampling;
the solvent delay time is 6 min;
temperature programming: maintaining at 50 deg.C for 1min, heating to 270 deg.C at 10 deg.C/min, and maintaining for 5 min;
the mass spectrum conditions of the gas chromatography-mass spectrometer are as follows:
ion source temperature: 230 ℃;
temperature of the quadrupole rods: 150 ℃;
an ionization mode: EI;
ionization energy: 70 eV;
mass scan range: 50-450 amu;
the measurement method comprises the following steps: SIM scanning;
the qualitative and quantitative ions for each component in the mass spectrum are shown in table 1.
| Name of Compound | Internal standard | Quantitative ion | Qualitative ion |
| 3-MCPD derivatives | D5-3-MCPD derivatives | 253 | 275/289/291 |
| D5-3-MCPD derivatives | 257 | 278/294/296 | |
| 2-MCPD derivatives | D5-2-MCPD derivatives | 253 | 75/289/291 |
| D5-2-MCPD derivatives | 257 | 79/294/296 | |
| 1, 3-DCP derivatives | D5-1, 3-DCP derivatives | 75 | 77/275/277 |
| D5-1, 3-DCP derivatives | 79 | 81/278/280 | |
| 2, 3-DCP derivatives | D5-2, 3-DCP derivatives | 75 | 77/111/253 |
| D5-2, 3-DCP derivatives | 79 | 81/116/257 |
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 testing the migration volume of chloropropanol and fatty acid ester in a packaging material is characterized by comprising the following steps: the testing method comprises the following steps:
1) preparing chloropropanol standard working solution (1 mg/L): weighing a certain amount of 3-MCPD, 2MCPD, 1, 3DCP and 2, 3-DCP, placing in a 100mL volumetric flask, adding n-hexane for dilution to scale, and mixing uniformly for later use;
2) preparing a deuterated chloropropanol standard working solution (10 mg/L): weighing a certain amount of D5Putting 3-MCPD, 2-MCPD, 1, 3-DCP and 2, 3-DCP in a l00mL volumetric flask, diluting to scale with n-hexane, and mixing for later use;
3) migration: taking a packaging material to be detected as a sample, and controlling the volume ratio of the surface area of the sample to the volume of the food simulation liquid to be 60cm2Soaking at a ratio of 100mL and preparing a migration liquid;
4) purifying: taking 10mL of migration liquid, adding an internal standard, mixing, adding the migration liquid into a diatomite solid-phase extraction column, standing for 10min, leaching with 20mL of n-hexane, discarding an effluent liquid, eluting with 30mL of ethyl acetate, collecting an eluent, blowing nitrogen to concentrate until the eluent is completely dried, dissolving residues with 2mL of n-hexane, transferring the dissolved residues into an l0mL glass tube with a plug, adding 5mL of anhydrous sodium sulfate, uniformly mixing, and dehydrating to form a purified liquid;
5) derivatization: adding 50 mu L of heptafluorobutyrylimidazole into the purified solution, carrying out vortex mixing for 30s, carrying out heat preservation at 70 ℃ for 120min, taking out, cooling to room temperature, adding 5mL of NaCl solution with the mass fraction of 20%, carrying out vortex mixing for 1min, and standing for layering; transferring the n-hexane phase, adding about 0.5g of anhydrous sodium sulfate for drying, and filtering by using a 0.22 mu m filter membrane to a sample injection vial to serve as a sample solution to be detected;
6) gas chromatography-mass spectrometry: adding the sample solution to be detected in the sample injection vial into a gas chromatography-mass spectrometer for gas chromatography-mass spectrometry;
7) and (3) qualitative confirmation: chromatographic peaks of the sample to-be-detected liquid and the known standard working solution appear at the same retention time, and the target analyte can be qualitatively confirmed at the moment;
8) quantitative analysis: and taking the concentration of each standard substance as an abscissa and the ratio of the response value of each quantitative chromatogram to the corresponding response value of the internal standard as an ordinate, making a linear regression equation of the standard curve, and comparing and quantifying the ratio of the response value of the sample to the response value of the corresponding internal standard with the standard curve.
2. The method for testing the migration amount of chloropropanol and fatty acid ester in a packaging material according to claim 1, characterized in that: the chromatographic conditions of the gas chromatography-mass spectrometer are as follows:
a chromatographic column: HP-5MS, column length 30m, internal diameter 0.25m, film thickness 0.25 m);
sample injection and carrier gas: helium gas;
flow rate: 2 mL/min;
sample inlet temperature: 220 ℃;
sample introduction amount: 1L, no shunt sampling;
the solvent delay time is 6 min;
temperature programming: maintaining at 50 deg.C for 1min, heating to 270 deg.C at 10 deg.C/min, and maintaining for 5 min;
the mass spectrum conditions of the gas chromatography-mass spectrometer are as follows:
ion source temperature: 230 ℃;
temperature of the quadrupole rods: 150 ℃;
an ionization mode: EI;
ionization energy: 70 eV;
mass scan range: 50-450 amu;
the measurement method comprises the following steps: and SIM scanning.
3. The method for testing the migration amount of chloropropanol and fatty acid ester in a packaging material according to claim 1, characterized in that: the temperature and time of the migrated soaking solution and soaking condition in the step 3) are selected according to GB31604.1-2015 and GB 5009.156-2016.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN115097022A (en) * | 2022-05-30 | 2022-09-23 | 浙江万盛股份有限公司 | Method for measuring content of impurities in process of preparing dichloropropanol by glycerol method |
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| CN103760290A (en) * | 2014-02-19 | 2014-04-30 | 常州进出口工业及消费品安全检测中心 | Method for measuring transfer volume of epoxy chloropropane in food contact material |
| CN110470756A (en) * | 2019-08-12 | 2019-11-19 | 华南理工大学 | The method and its application of the organic chloro thing DCP content of nocuousness of PAE wet strength agent in a kind of measurement paper for daily use |
| CN112098547A (en) * | 2020-09-01 | 2020-12-18 | 深圳天祥质量技术服务有限公司 | Specific migration method for measuring 1, 3-dichloro-2-propanol and 3-chloro-1, 2-propanediol in paper material |
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Patent Citations (3)
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| CN103760290A (en) * | 2014-02-19 | 2014-04-30 | 常州进出口工业及消费品安全检测中心 | Method for measuring transfer volume of epoxy chloropropane in food contact material |
| CN110470756A (en) * | 2019-08-12 | 2019-11-19 | 华南理工大学 | The method and its application of the organic chloro thing DCP content of nocuousness of PAE wet strength agent in a kind of measurement paper for daily use |
| CN112098547A (en) * | 2020-09-01 | 2020-12-18 | 深圳天祥质量技术服务有限公司 | Specific migration method for measuring 1, 3-dichloro-2-propanol and 3-chloro-1, 2-propanediol in paper material |
Non-Patent Citations (3)
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| 胡启立 等: "固相萃取-同位素内标-气相色谱-质谱法测定纸质食品接触材料中 4 种氯丙醇的迁移量", 分析化学, vol. 48, no. 10, pages 1434 - 1436 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115097022A (en) * | 2022-05-30 | 2022-09-23 | 浙江万盛股份有限公司 | Method for measuring content of impurities in process of preparing dichloropropanol by glycerol method |
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