Quantification of Phthalate Leaching from Food Contact Materials by GC/MS

Significance of the Topic

Migration of compounds from food contact materials into food can degrade quality and pose health risks. Phthalates, widely used as plasticizers, are of particular concern due to potential endocrine-disrupting effects. Regulatory limits demand robust analytical methods to monitor phthalate leaching and ensure compliance with EU directives.

Objectives and Study Overview

This application note evaluates a GC/MS method for quantifying three regulated phthalates (DBP, BBP, DEHP) and three common phthalates (DMP, DEP, DnOP) leached from various plastic food contact materials. It employs Selected Ion Full Scan (SIFI) mode on a PerkinElmer Clarus SQ 8 GC/MS to achieve high sensitivity for target analytes while simultaneously screening for unknown leachables. The impact of temperature and food simulant composition on migration is investigated.

Methodology

Samples of PTFE bottles, PVC cling film, PET trays, and PP bottles were exposed to food simulants (10% ethanol, 3% acetic acid, 20% ethanol) under accelerated conditions (10 days at 20 °C and 50 °C; microwavable test at 100 °C for one hour). Following exposure, phthalates were extracted with n-hexane, concentrated fivefold, and analyzed by GC/MS. Spike recovery tests assessed extraction efficiency, and external calibration standards spanned low and high concentration ranges to cover regulatory limits.

Used Instrumentation

• PerkinElmer Clarus 680 GC with Elite-5 MS capillary column (30 m × 0.25 mm × 0.25 μm)
• Programmable split/splitless injector at 280 °C and 5 μL autosampler
• PerkinElmer Clarus SQ 8C MS in SIFI mode (EI ionization, scan range m/z 45–400)

Main Results and Discussion

• Calibration curves for all six phthalates showed strong linearity (R² > 0.994) and repeatability (RSD < 4%).
• Spike recoveries were 83–107% for most phthalates; DMP exhibited lower recoveries (46–57%) due to its higher polarity.
• PVC cling film was the only material with detectable phthalate migration. Elevated temperatures and lipophilic simulants (20% ethanol) significantly increased leaching compared to aqueous or acidic media.

Benefits and Practical Applications

This SIFI GC/MS method provides reliable quantification of regulated and common phthalates in food packaging. It supports regulatory compliance, quality control, and simultaneous detection of unknown leachables, enhancing safety monitoring in the food industry.

Future Trends and Potential Applications

• Adoption of high-resolution mass spectrometry to broaden screening for unknown contaminants.
• Streamlined sample preparation to improve laboratory throughput.
• Extension of the approach to novel packaging materials and emerging alternative plasticizers under evolving regulations.

Conclusion

The PerkinElmer Clarus SQ 8 GC/MS in SIFI mode delivers high sensitivity, accuracy, and repeatability for phthalate migration testing. Results confirm that temperature and simulant composition critically affect leaching, underscoring the importance of realistic test conditions for ensuring food safety.

Reference

1. C.A. Staples. Phthalate Esters. In The Handbook of Environmental Chemistry; Springer, 2003.
2. Commission Regulation (EU) No 10/2011 on plastic materials and articles intended to come into contact with food; Official Journal of the European Union.
3. European Chemicals Agency. Guidance on phthalate restrictions; ECHA, 2016.
4. L. Nollet. Handbook of Food Analysis: Residues and Other Food Component Analysis; Marcel Dekker, 2004.