Quantitative screening of possible migrants from paperboard packaging material by solid-phase micro extraction coupled to gas chromatography-mass spectrometry

Significance of the topic

In food packaging, paperboard materials can release migrants such as phthalates, phenols and off-flavor compounds that pose risks for food safety and consumer health.
Reliable and efficient screening methods are essential for quality control and regulatory compliance.

Objectives and Study Overview

This study aimed to develop and validate a fully automated, quantitative screening method for 12 representative migrants from paperboard using solid-phase micro extraction coupled to GC–MS/MS.
The method targets phthalates, photoinitiators, phenolic antioxidants and volatile off-flavor compounds.

Methodology and Instrumentation

Sample preparation:

• Paperboard pieces (2×2 mm) spiked and placed in headspace vials with 13% methanol in water solution
• Extraction using 100 μm PDMS SPME fiber at 65 °C for 45 min
• Desorption in GC injector at 270 °C for 7 min

Instrumental setup:

• Thermo Scientific TSQ 8000 triple-stage quadrupole MS coupled to a Trace 1310 GC
• TriPlus RSH autosampler for automated SPME handling
• TG-5 SilMS column (0.25 mm × 30 m, 0.25 μm)
• Electron ionization at 70 eV in positive SRM mode

Main Results and Discussion

Validation results for 12 analytes showed:

• Recoveries between 77% and 118%
• Repeatability (RSD) below 22%
• LODs in the sub-μg/kg to μg/kg range, LOQs suitable for regulatory limits

Survey of 12 paperboard samples (virgin vs. recycled, printed vs. unprinted) revealed higher migrant levels in recycled and printed materials, confirming method sensitivity in real matrices.

Benefits and Practical Applications

The automated SPME–GC–MS/MS workflow:

• Eliminates solvent use and reduces sample handling
• Offers high throughput and reproducibility
• Is robust for routine quality control in food contact material laboratories

Future Trends and Potential Applications

Opportunities include:

• Extension to non-target and suspect screening using high-resolution MS
• Integration of complementary extraction techniques (e.g., SBSE, TFME)
• Miniaturization and on-site testing solutions
• Implementation of data-driven analytics and AI for screening and risk assessment

Conclusion

The developed and validated automated SPME–GC–MS/MS method provides a rapid, sensitive and reliable quantitative screening tool for key migrants in paperboard packaging materials, supporting food safety monitoring and regulatory compliance.