Lipase-assisted matrix clean-up for robust and simultaneous determination of 12 novel brominated flame retardants in marine biota: a case study in squid

초록

Novel brominated flame retardants (NBFRs) present environmental and health risks. This study proposes an analytical method for simultaneously detecting 12 NBFRs in squid. Squid was selected as a representative lipid-rich marine matrix to validate the method. Existing methods utilize acidified silica columns for sample preparation, which degrades certain NBFR compounds and limits detection. The proposed method uses lipase-based lipid hydrolysis, which effectively eliminates fat without degrading target compounds and enables simultaneous analysis of all 12 NBFRs. Further, gas chromatography (GC) coupled with electron impact ionization-tandem mass spectrometry is employed for sensitive and selective analyses. We have selected a high-temperature resistant GC column that demonstrates enhanced sensitivity for less volatile compounds such as OBIND and DBDPE. The proposed analytical method was rigorously validated in accordance with the CODEX guidelines (CAC/GL 71-2009); it demonstrated excellent performance in terms of selectivity, linearity, recovery, accuracy, precision, limit of detection, and limit of quantification. This study lays the foundation for a robust marine monitoring strategy for managing contaminants like NBFRs.

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