Evaluation of analytical performance of gas chromatography coupled with atmospheric pressure chemical ionization Fourier transform ion cyclotron resonance mass spectrometry (GC-APCI-FT-ICR-MS) in the target and non-targeted analysis of brominated and chlorinated flame retardants in food.

A new analytical method was established and validated for the analysis of eighteen halogenated flame retardants (HFRs)in food products. Gas chromatography (GC) coupled to Fourier transform ion cyclotron resonance mass spectrometry (FT-ICR-MS) employing atmospheric pressure chemical ionization (APCI) was used for the identification and quantitation of contaminants. Intra-laboratory validation of the method was performed with respect to recovery, repeatability, linear calibration ranges, instrumental and method limits of quantitation (i-LOQ and m-LOQ), and trueness was verified where possible by analysis of reference materials (RMs). The validation results indicated recoveries of analytes between 59 and 115%, the repeatability in terms of relative standard deviations (RSDs) in the range of 5-15% and linearity with correlation coefficients of ≥0.99 between the i-LOQ and 250 pg injected on-column. The method i-LOQs ranged from ∼1 pg to ∼5 pg injected on-column, while m-LOQs were in the range of 0.002-0.04 ng g sample. The measured values for RMs agreed with the provided values, giving the accuracy of obtained concentrations in the range of 92-133% with RSD range of 2-15% and were in agreement with the results obtained with the reference method based on magnetic sector GC-HRMS. For the majority of the compounds, the method met a limit of quantification criterion stated in the Commission Recommendation, 2014/118/EU on monitoring BFRs in food. The developed method was demonstrated to be suitable for qualitative screening of suspect target contaminants presented in the samples by the post-run treatment of raw data and confirmation by isotope cluster analysis.