Multiresidual Determination - Validating Specific Migrations from Packaging into Food Simulant Using LC-MS/MS

Significance of the topic

Migration of monomers and additives from plastic packaging into food is a critical safety concern. Substances such as terephthalic acid, bisphenols and photo-initiators can transfer into food during storage and processing, potentially exceeding regulatory specific migration limits and posing health risks.

Objectives and study overview

This work aimed to develop and validate a rapid, sensitive UHPLC-MS/MS method for simultaneous quantification of five target migrants—terephthalic acid (PTA), isophthalic acid (i-PTA), bisphenol S (BPS), bisphenol A (BPA), and benzophenone (BP)—using orthophthalic acid as an internal standard in a 50 % ethanol food simulant.

Methodology and instrumentation

The analytical separation employed an Agilent 1290 Infinity UHPLC with a ZORBAX Eclipse Plus C18 column (2.1 × 100 mm, 1.8 µm) and a binary gradient of methanol and 0.1 % acetic acid in water. Detection was achieved on an Agilent 6460 Triple Quadrupole MS with Jet Stream ESI in both positive and negative MRM modes. Standard solutions (60–1,000 µg/kg) and spiked simulant (50 % ethanol v/v) were used to establish linearity, limits of detection (LOD) and quantification (LOQ), precision (repeatability and intermediate), and recovery following a 24 h contact at 40 °C.

Main results and discussion

• Chromatographic run time: 8 minutes for all analytes including the internal standard.
• LODs ranged from 1.9 µg/kg (BPS) to 12.6 µg/kg (BPA), and LOQs from 5.9 to 40.2 µg/kg, exceeding regulatory sensitivity requirements by factors of 50–1,923.
• Calibration was linear with R² values ≥ 0.992 across the tested ranges.
• Repeatability RSDs were between 1 % and 9 %; intermediate precision RSDs remained within 3 % to 15 %, except BP at 23 % for the highest level.
• Recoveries ranged from 89 % to 112 %, meeting accepted guidelines.

Benefits and practical applications

This multiresidue UHPLC-MS/MS approach reduces analysis time and solvent consumption compared to individual methods prescribed by EN standards. It supports regulatory compliance for specific migration testing in QA/QC laboratories handling diverse packaging materials and coatings.

Future trends and possibilities

Extension of this method to additional non-intentionally added substances (NIAS), emerging plasticizers, and higher-resolution mass analyzers could further broaden screening capabilities. Integration with automated sample preparation and data processing will streamline routine surveillance workflows.

Conclusion

The presented UHPLC-MS/MS method is fast, robust, and compliant with European and Mercosur specific migration limits. It offers reliable simultaneous quantification of key packaging migrants in food simulants, facilitating efficient monitoring of material safety.

Reference

• Fávaro M.Â., Padula M., Daniela D. Multiresidual Determination Validating Specific Migrations from Packaging into Food Simulant Using LC-MS/MS. Agilent Technologies Application Note, 2017.
• European Commission. Regulation (EU) No 10/2011 on plastic materials and articles in contact with food.
• Grupo Mercado Comum. GMC/Res. 02/12: Positive list of monomers for food contact plastics. Mercosur, 2012.