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GC-MS/MS (gas chromatography-mass spectrometer/mass spectrometer) technique-based method for analyzing migration volume from photoinitiator to MPPO (modified polyphenylene oxide) in printing packaging paper

A technology of photoinitiator and technical analysis, applied in the direction of analysis of materials, measurement devices, material separation, etc., can solve the problem of no photoinitiator specific migration analysis method

Active Publication Date: 2014-05-28
CHINA NAT TOBACCO QUALITY SUPERVISION & TEST CENT
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, domestic research mainly focuses on the detection of photoinitiator residues in food or packaging materials, and rarely involves the analysis of the specific migration of photoinitiators in dry foods, let alone the use of MPPO as a simulant for the specific migration of photoinitiators. report on analytical methods

Method used

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  • GC-MS/MS (gas chromatography-mass spectrometer/mass spectrometer) technique-based method for analyzing migration volume from photoinitiator to MPPO (modified polyphenylene oxide) in printing packaging paper
  • GC-MS/MS (gas chromatography-mass spectrometer/mass spectrometer) technique-based method for analyzing migration volume from photoinitiator to MPPO (modified polyphenylene oxide) in printing packaging paper
  • GC-MS/MS (gas chromatography-mass spectrometer/mass spectrometer) technique-based method for analyzing migration volume from photoinitiator to MPPO (modified polyphenylene oxide) in printing packaging paper

Examples

Experimental program
Comparison scheme
Effect test

example 1

[0033] 1. Instruments and reagents:

[0034] 18 photoinitiators: 2-hydroxy-2-methyl-1-phenylacetone, methyl benzoylformate, benzophenone, 2-methylbenzophenone, 1-hydroxycyclohexylphenylmethanone Ketone (photoinitiator 184), ethyl p-N,N-dimethylaminobenzoate, 3-methylbenzophenone, 4-methylbenzophenone, 2,2-dimethoxy-2 -Phenylacetophenone (benzoin dimethyl ether), methyl phthaloylbenzoate, isooctyl p-dimethylaminobenzoate, 2-methyl-1-(4-methylthio)phenyl 2- Morpholinyl-1-propanone (photosensitizer 907), 4-isopropylthioxanthone, 2-isopropylthioxanthone, biphenylbenzophenone, 2,4-diethylthioxanthone Ketone (photoinitiator DETX), 4,4-bis(dimethylamino)benzophenone (Michler's ketone), 4,4-bis(diethylamino)benzophenone (tetraethylmichler's ketone) , internal standard: deuterated anthracene, all analytically pure; acetonitrile, acetone, n-hexane, ethyl acetate, methanol, all chromatographic grade reagents; distilled water, in line with the requirements of first-grade water in GB / T ...

example 2

[0055] As described in Example 1, transfer the modified polyphenylene ether simulant that has completed the migration experiment into a centrifuge tube with a stopper, add 10 mL of acetonitrile extractant, and take different vortex times (namely 2min, 5min, 7min and 10min) for one time Extraction and two extractions, compare the difference in the extraction effect of 70 ° C water bath for 24 hours, the extract was dried and reconstituted, filtered for GC-MS / MS analysis. The differences in the extraction effects of different vortex extraction times compared with 70°C water bath for 24 hours were all within plus or minus 10%, and the differences in the extraction effects of vortex extraction once and twice compared with 70°C water bath for 24 hours were mostly within 10%. Then use 10min vortex extraction once to achieve the purpose of extraction.

[0056]

example 3

[0058] As can be seen from Example 1, since the minimum limit of the photoinitiator involved is 0.01 mg / kg, which fully meets the sensitivity requirements of the method, 1 g MPPO can be used in the pretreatment process instead of 4 g MPPO in the EU standard. Since MPPO is expensive and the recycling process is cumbersome, reducing the amount of MPPO used in the pretreatment process also reduces the cost under the premise of meeting the sensitivity requirements. This example compares the area of ​​the packaging sample used in the migration experiment with the mass ratio of the modified polyphenylene ether simulant, respectively 1dm 2 : 4g and 0.25dm 2 : the amount of migration in two situations of 1g, the experimental results are shown in Table 4, as can be seen from the experimental results, there is no significant difference in the ratio of two kinds of migration experiments, and this method can be used to use the area and modification of the packaging samples for migration...

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Abstract

The invention discloses a GC-MS / MS (gas chromatography-mass spectrometer / mass spectrometer) technique-based method for analyzing the migration volume from a photoinitiator to MPPO (modified polyphenylene oxide) in printing packaging paper. The method is characterized in that a photoinitiator target released by a sample under a simulated condition is adsorbed by MPPO, and a solvent is extracted from the MPPO by acetonitrile, and supernate is concentrated and then is filtered so as to determine the specific migration volume of the photoinitiator in a printing packaging material by the GC-MS / MS method. The method can be rapidly and accurately used for detecting the specific migration volume of the photoinitiator in the printing packaging material, has an accurate determination result, is good in repeatability, is simple in pretreatment process, and is low in detection and analysis cost.

Description

technical field [0001] The invention belongs to the technical field of detecting specific migration of photoinitiators to modified polyphenylene ether simulants in printing and packaging materials, and mainly relates to 2-hydroxy-2-methyl-1-phenylacetone and benzoyl in printing and packaging materials Methyl formate, benzophenone, 2-methylbenzophenone, 1-hydroxycyclohexyl phenyl ketone (photoinitiator 184), ethyl p-N,N-dimethylaminobenzoate, 3- Methylbenzophenone, 4-methylbenzophenone, 2,2-dimethoxy-2-phenylacetophenone (benzoin dimethyl ether), methyl phthaloylbenzoate, p-dimethoxy Isooctyl methylaminobenzoate, 2-methyl-1-(4-methylthio)phenyl 2-morpholinyl-1-propanone (photosensitizer 907), 4-isopropylthioxanthone, 2 -Isopropylthioxanthone, biphenylbenzophenone, 2,4-diethylthioxanthone (photoinitiator DETX), 4,4-bis(dimethylamino)benzophenone (m ketone), 4,4-bis (diethylamino) benzophenone (tetraethyl Michler's ketone) and other 18 kinds of photoinitiator specific migration...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02G01N30/06
Inventor 刘珊珊李中皓杨飞范子彦边照阳王颖张艳革张洪非唐纲岭胡清源
Owner CHINA NAT TOBACCO QUALITY SUPERVISION & TEST CENT
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