MONITORING OF BISPHENOL A AND ITS ANALOGUES IN ENVIRONMENTAL MATRICES USING THE AGILENT 6550 Q-TOF LC/MS

Importance of the Topic

Bisphenols such as BPA and its analogues are widely used in plastics and resins and can leach into the environment, posing health and ecological risks due to their endocrine-disrupting properties. Monitoring these compounds in various environmental matrices is essential to assess contamination levels, regulatory compliance, and potential bioaccumulation, especially in sensitive ecosystems.

Study Objectives and Overview

This study, initiated by the Norwegian Environment Agency, aimed to screen and quantify BPA, BPF (both 4,4’- and 2,2’- isomers), BPAF, BP-BP, and BPS in effluent, sludge, leachate, sediment and biological samples from marine and freshwater environments. The goal was to evaluate their occurrence, distribution, and bioaccumulation potential using high-resolution mass spectrometry.

Methodology and Instrumentation

Sample preparation workflows were tailored to each matrix:

• Water: Solid-phase extraction on PPL cartridges, elution with methanol/acetonitrile and acetone, concentration and reconstitution.
• Sediment and sludge: Accelerated solvent extraction with diatomaceous earth, followed by multimode SPE cleanup.
• Biological samples: Ultrasonic extraction with dichloromethane, liquid-liquid partition (n-hexane/acetonitrile), and cleanup with Florisil and PSA/C18 dSPE.

Instrumentation details:

• UHPLC: Agilent 1290 Infinity with Biphenyl column, methanol/water mobile phase, 10 min runtime.
• Mass spectrometry: Agilent 6550 Q-TOF MS with Dual Jet Stream ESI in negative mode, accurate mass acquisition, internal standard (13C-BPA), data processed in MassHunter.

Key Results and Discussion

• Effluent and Sludge: Wastewater treatment plants were confirmed as significant sources of various bisphenols, with detectable levels in effluent and biosolids.
• Leachate: Landfill leachate contained BPA, BPF, BP-BP and BPS, indicating persistence in solid waste environments.
• Sediment: BPF and BPA accumulated in both marine (Oslofjord) and freshwater (Lake Mjøsa) sediments receiving treated effluent.
• Biota: Northern shrimp and perch from contaminated sites showed bioaccumulation of all target bisphenols, highlighting food chain transfer.

Benefits and Practical Applications

• The Q-TOF LC/MS approach offers high sensitivity, accurate mass data for retrospective screening of additional bisphenols in stored samples.
• Robust sample preparation protocols enable reliable quantification across diverse environmental and biological matrices.
• Data support risk assessment, regulatory monitoring, and inform pollution mitigation strategies in aquatic systems.

Future Trends and Applications

Emerging needs include expanding the screening scope to novel bisphenol analogues and transformation products, integrating non-target and suspect screening workflows, and coupling high-resolution MS with machine learning for contaminant profiling. Longitudinal studies and biomonitoring will improve understanding of temporal and spatial trends in bisphenol exposure.

Conclusion

The use of Agilent 6550 Q-TOF LC/MS demonstrated a comprehensive, sensitive platform for surveying bisphenols in complex environmental samples. The findings confirm widespread distribution and bioaccumulation potential of BPA and its analogues, underlining the necessity for continued monitoring and regulatory evaluation.

Reference

1. European Commission. Commission Regulation (EU) No 10/2011 on plastic materials and articles in contact with food.
2. European Commission. Commission Directive 2011/8/EU amending Directive 2002/72/EC on restriction of BPA in infant feeding bottles.
3. European Food Safety Authority (EFSA). Press Release: Bisphenol A risk assessment consultation, 17 January 2014.
4. Norwegian Environment Agency. Screening Program 2013 report M-176/2014: New bisphenols and emerging contaminants, Thomas et al.