High-throughput non-targeted screening method for pollutants in regenerated PET material for food contact

A food contact and contaminant technology, applied in the direction of material separation, analytical materials, measuring devices, etc., can solve the problem of unrelated standards or methods of recycled PET, systemic risk monitoring and assessment of PET for difficult food contact, non-recycling PET and other problems, to achieve the effects of rapid sensitivity and selectivity, recycling and reuse, strong safety risk assessment, and high accuracy

Pending Publication Date: 2022-01-07
TECH CENT OF GUANGZHOU CUSTOMS
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Recycled PET has not been allowed to be used in food contact materials due to concerns that the source of the contaminants in recycled PET is unknown and may lead to food safety risks; there are no normative standards or methods for the determination of NIAS / IAS in recycled PET
The lack of methods makes it difficult to carry out systematic risk monitoring and assessment of PET for food contact. It is very difficult to identify NIAS detected in recycled PET. Many NIAS substances, especially non-volatile organic pollutants, do not have standard substances or not included in any available database

Method used

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  • High-throughput non-targeted screening method for pollutants in regenerated PET material for food contact
  • High-throughput non-targeted screening method for pollutants in regenerated PET material for food contact
  • High-throughput non-targeted screening method for pollutants in regenerated PET material for food contact

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Experimental program
Comparison scheme
Effect test

preparation example Construction

[0034] Preparation of uniform and stable samples: Take an appropriate amount of recycled PET bottle flakes and grind them in a high-speed rotary grinder, and use them as samples for condition optimization and testing.

[0035] Weigh 0.2g to 1.0g of the sample to be tested in a clean glass bottle, add an appropriate amount of HFIP to dissolve the polymer, and when it is completely dissolved, add methanol and ultrasonicate for 1 hour to completely precipitate the polymer. Subsequently, the mixture was centrifuged at 9000 rpm for 10 min, the supernatant was taken, the wall of the centrifuge tube and the residual precipitate were washed with 1 mL of methanol, and the obtained supernatants were combined. Blow the supernatant to near dryness under gentle nitrogen flow or rotary evaporation, and redissolve with 1 mL of methanol. The reconstituted solution was filtered through a 0.22 μm filter to obtain the sample to be tested. Two parallels were set up for each sample, and a blank s...

Embodiment 1

[0051] Embodiment 1: the optimization of the method for measuring non-volatile organic pollutants

[0052] 1. Optimization of the pretreatment method

[0053] The sample pretreatment method was optimized by testing the native PET sample spiked recovery rate (50 μL 10 mg / L BBP-D4).

[0054]1.1 Selection of Precipitation Solvent Precipitation solvent is one of the important factors affecting pretreatment efficiency. If precipitation occurs too quickly, it is easy to wrap the substance to be tested; if precipitation occurs slowly or no precipitation occurs, a large amount of solvent will be consumed, which will increase The expenditure also reduces the test efficiency. The experiment investigated the effect of several common solvents (acetone, methanol, n-hexane) on the recovery rate of BBP-D4 spiked. The results are shown in Table 1 below. When methanol was used as the reprecipitation solvent, the recovery rate of the standard addition was the highest. This is because when me...

Embodiment 2

[0076] Embodiment 2: the optimization of the method for measuring volatile organic pollutants

[0077] 2.1 Method optimization

[0078] GC×GC-QTOF-MS was used to optimize the equilibration time, solid phase microextraction temperature, solid phase microextraction fiber head type, oven heating rate and modulation cycle, and the total area of ​​chromatographic peaks and the number of chromatographic peaks were used as the basis for optimization.

[0079] The headspace equilibration time was selected as 15min, 30min and 60min for comparison, the extraction temperature was selected as 50°C, 70°C, 90°C, 110°C, 130°C and 150°C for comparison, and three different types of solid phase microextraction fiber heads were compared ( 100μmPDMS, 65μmDVB / PDMS and 80μmDVB / C-WR / PDMS) extraction effects, in terms of instrument optimization, the separation effects of four heating rates of 3°C / min, 5°C / min, 8°C / min and 10°C / min were compared , and compared the peaking effects of three modulation ...

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Abstract

The invention discloses a high-throughput non-targeted screening method for pollutants in a regenerated PET (Polyethylene Terephthalate) material for food contact. Ultra-high performance liquid chromatography-quadrupole time-of-flight high-resolution mass spectrometry (UPLC-QTOF-MS), SPME-GC x GC-QTOF-MS and GC x GC-QTOF-MS to screen the pollutants in recycled PET bottle chips for food contact, wherein the pollutants comprise non-volatile organic pollutants, volatile organic pollutants and semi-volatile organic pollutants. The method has the advantages of high throughput, high accuracy, rapidness, sensitivity, good selectivity and the like.

Description

Technical field: [0001] The invention relates to the technical field of food safety detection, in particular to a high-throughput non-targeted screening method for pollutants in recycled PET materials for food contact. Background technique: [0002] Polyethylene terephthalate (PET) has good air permeability, gloss, stability and formability, and is widely used in food packaging. At present, PET bottles have ranked first in the field of plastic food packaging. However, PET is a non-biodegradable material, which is easy to cause serious environmental pollution and waste of resources. Therefore, the recycling of PET food packaging has become a major measure to solve plastic waste and protect ecological safety at home and abroad, and has a huge development prospect. [0003] However, the chemicals and contaminants of recycled PET materials for food packaging are more complex than those of virgin PET materials. On the one hand, because there are different types of chemical sub...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/06G01N30/88
CPCG01N30/06G01N30/88
Inventor 董犇钟怀宁李丹陈胜吴学峰寇筱雪吴思亮李函珂黎梓城郑建国
Owner TECH CENT OF GUANGZHOU CUSTOMS
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