The Analysis of Bisphenol A-diglycidyl Ether (badge), Bisphenol F-diglycidyl Ether (bfdge) and Their Derivatives in Canned Food and Beverages by LC-MS/MS

Importance of the topic

Monitoring the migration of bisphenol A-diglycidyl ether (BADGE), bisphenol F-diglycidyl ether (BFDGE) and their transformation products from epoxy-coated cans into food and beverages is critical for consumer safety and regulatory compliance. These compounds and their derivatives may exhibit mutagenic, genotoxic, or endocrine-disrupting effects, and specific migration limits are enforced by the European Union to ensure food safety.

Goals and overview of the study

The primary objective was to develop and validate a rapid, sensitive, and robust liquid chromatography–tandem mass spectrometry (LC-MS/MS) method for simultaneous quantification of BADGE, BFDGE, and a range of hydrolyzed and chlorinated derivatives in canned food and beverage matrices. Application to real samples aimed to demonstrate method suitability for routine quality control.

Methodology and instrumentation

Sample Preparation:

• Beverages: Sonicate 20 mL sample for 20 min, load 3 mL onto conditioned polymeric SPE cartridge, elute with methanol, evaporate, reconstitute in MeOH/H₂O (1:1), filter, and inject 10 µL.
• Canned food: Homogenize 3 g sample with ethyl acetate, shake and sonicate, centrifuge, evaporate 5 mL supernatant, reconstitute in MeOH/H₂O (1:1), filter, and inject 10 µL.

Chromatography:

• Column: Fused Core™ Ascentis Express C18, 150×2.1 mm, 2.7 µm.
• Mobile phase: 25 mM formate buffer (pH 3.75, 50 °C) and methanol.
• Gradient: 30→50% B (0.75 min), 50→60% B (0.5 min), 60→80% B (4 min), hold 0.5 min.
• Flow rate: 600 µL/min.

Mass Spectrometry:

• Instrument: Thermo Scientific TSQ Quantum Ultra triple quadrupole with heated ESI (positive mode).
• Key settings: spray voltage 4 kV; vaporizer 475 °C; capillary 375 °C; sheath/auxiliary gas 60/40 units; collision gas Ar 1.5 mTorr.

Main results and discussion

The method achieved method limits of quantification ranging from 0.13 to 1.6 µg/L in beverages and 1.0 to 4.0 µg/kg in food. Calibration exhibited excellent linearity (r² > 0.999) over 0.5–5 000 µg/kg. Precision (RSD) was below 20% at low levels and below 11% at medium levels. Recoveries ranged from 60% to 95%.
Analysis of seven beverage and six canned food samples revealed:

• BADGE·2H₂O detected in all matrices at 2.3–5.1 µg/L (drinks) and 2.7–675 µg/kg (foods).
• Other BADGE derivatives (hydrolyzed and chlorinated) quantified in food; parent BADGE and BFDGE species were absent in aqueous samples, likely due to hydrolysis and reduced usage of BFDGE-based coatings.

Benefits and practical applications

This LC-MS/MS approach provides a fast, sensitive, and reliable tool for routine surveillance of epoxy resin migrants in the food industry. It supports compliance with EU specific migration limits, enables quality control in production, and helps assess consumer exposure.

Future trends and possibilities

Advances may include high-resolution mass spectrometry for non-target screening of unknown migrants, microflow LC for reduced solvent consumption, automated sample preparation, and expansion to other packaging-related contaminants. Integration with data analytics could enhance rapid risk assessment.

Conclusion

A validated LC-MS/MS method was established for simultaneous determination of BADGE, BFDGE, and their derivatives in canned foods and beverages. The procedure combines straightforward sample preparation, fast chromatographic separation, and sensitive detection. Application to real samples confirmed its suitability for food safety monitoring and regulatory compliance.

Reference

Gallart-Ayala H, Moyano E, Galceran MT. J Chrom A. 2011;1218:12.
Commission Directive 2002/16/EC. Use of epoxy derivatives in food contact materials.
Commission Regulation (EC) No 1895/2005. Restriction of certain epoxy derivatives in food contact materials.
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