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 pose risks to product quality and human health Phthalates used as plasticisers are prone to leaching and are restricted due to endocrine disruptions This study addresses the need for accurate quantification of phthalate migration in compliance with EU regulation No 10 2011

Objectives and Study Overview

The work aims to develop a reliable gas chromatography mass spectrometry approach using Selected Ion Full Ion mode to quantify regulated and common phthalates including DEHP DBP BBP DMP DEP and DnOP in food simulants The effects of temperature time and simulant composition on leaching from various plastic food packaging types are also investigated

Methodology and Instrumentation

Sample preparation followed EU No 10 2011 using three simulants 10 percent ethanol 3 percent acetic acid and 20 percent ethanol Plastics were exposed under accelerated conditions and microwavable samples were tested at room temperature and at 100 degrees Celsius One hour exposures simulated high temperature use Extraction employed n hexane with salt induced phase separation followed by concentration to assess phthalate levels Calibration used external standards spanning 0.2 to 200 mg per liter

Instrumentation Used

PerkinElmer Clarus 680 gas chromatograph with Elite 5 MS capillary column 30 meters by 0.25 millimeter by 0.25 micrometer Programmable split splitless injector at 280 degrees Celsius Helium carrier gas at constant pressure PerkinElmer Clarus SQ 8C mass spectrometer operated in Selected Ion Full Ion mode Electron impact ionisation at 280 degrees Celsius source temperature Scan range m per z 45 to 400 with simultaneous selected ion monitoring for targeted phthalate ions

Main Results and Discussion

External calibration curves for six phthalates showed excellent linearity with R squared values above 0.994 Spike recoveries ranged from 83 to 107 percent except for DMP which showed lower extraction due to polarity differences Temperature elevation increased phthalate migration particularly for cling film Samples in 20 percent ethanol exhibited the highest leaching followed by 10 percent ethanol and acetic acid Unknown low intensity peaks detected by full scan suggest the presence of additional leachables under defined conditions

Benefits and Practical Applications

The method enables simultaneous targeted quantification and non targeted screening in a single run offering high sensitivity and repeatability It supports compliance testing for food contact materials quality control and safety assessment in research and industrial laboratories

Future Trends and Applications

Emerging developments include integration of high resolution mass spectrometry workflows for improved identification of unknown migrants miniaturised sample preparation using microextraction or solid phase techniques and adoption of green solvents Further work may extend to other additive classes and real food matrices under dynamic storage scenarios

Conclusion

The presented GC MS approach provides a robust solution for monitoring phthalate migration from food contact materials under regulatory conditions offering high accuracy and operational efficiency

References

• Staples C A 2003 Phthalate Esters The Handbook of Environmental Chemistry Springer
• Commission Regulation EU No 10 2011 of 14 January 2011 on Plastic Materials and Articles Intended to Come into Contact with Food Official Journal of the European Union
• European Chemicals Agency 2016 Guidance on Phthalate Regulation Accessed 24 June 2016
• Nollet L 2004 Handbook of Food Analysis Residues and Other Food Component Analysis Volume 2 Marcel Dekker