Multi-class, multi-residue analysis of pesticides, polychlorinated biphenyls, polycyclic aromatic hydrocarbons, polybrominated diphenyl ethers and novel flame retardants in fish using fast, low-pressure gas chromatography–tandem mass spectrometry

A multi-class, multi-residue method for the analysis of 13 novel flame retardants, 18 representative pesticides, 14 polychlorinated biphenyl (PCB) congeners, 16 polycyclic aromatic hydrocarbons (PAHs), and 7 polybrominated diphenyl ether (PBDE) congeners in catfish muscle was developed and evaluated using fast low pressure gas chromatography triple quadrupole tandem mass spectrometry (LP-GC/MS–MS). The method was based on a QuEChERS (quick, easy, cheap, effective, rugged, safe) extraction with acetonitrile and dispersive solid-phase extraction (d-SPE) clean-up with zirconium-based sorbent prior to LP-GC/MS–MS analysis. The developed method was evaluated at 4 spiking levels and further validated by analysis of NIST Standard Reference Materials (SRMs) 1974B and 1947. Sample preparation for a batch of 10 homogenized samples took about 1 h/analyst, and LP-GC/MS–MS analysis provided fast separation of multiple analytes within 9 min achieving high throughput. With the use of isotopically labeled internal standards, recoveries of all but one analyte were between 70 and 120% with relative standard deviations less than 20% (n = 5). The measured values for both SRMs agreed with certified/reference values (72–119% accuracy) for the majority of analytes. The detection limits were 0.1–0.5 ng g−1 for PCBs, 0.5–10 ng g−1 for PBDEs, 0.5–5 ng g−1 for select pesticides and PAHs and 1–10 ng g−1 for flame retardants. The developed method was successfully applied for analysis of catfish samples from the market.

Graphical abstractFigure optionsDownload full-size imageDownload as PowerPoint slideHighlights► A method for analysis of POPs and novel flame retardants in catfish was developed. ► The method is based on a QuEChERS extraction, d-SPE clean-up and low pressure GC/MS–MS. ► The method validation demonstrated good recoveries and low detection limits. ► The method was successfully applied for analysis of catfish samples from the market.