PMID- 26526911 OWN - NLM STAT- PubMed-not-MEDLINE DCOM- 20160202 LR - 20151103 IS - 1873-4324 (Electronic) IS - 0003-2670 (Linking) VI - 898 DP - 2015 Oct 22 TI - Analytical capabilities of high performance liquid chromatography - Atmospheric pressure photoionization - Orbitrap mass spectrometry (HPLC-APPI-Orbitrap-MS) for the trace determination of novel and emerging flame retardants in fish. PG - 60-72 LID - S0003-2670(15)01242-8 [pii] LID - 10.1016/j.aca.2015.10.008 [doi] AB - A new analytical method was established and validated for the analysis of 27 brominated flame retardants (BFRs), including so called "emerging" and "novel" BFRs (EBFRs and NBFRs) in fish samples. High performance liquid chromatography (HPLC) coupled to Orbitrap mass spectrometry (Orbitrap-MS) employing atmospheric pressure photoionization (APPI) interface operated in negative mode was used for the identification/quantitation of contaminants. HPLC-Orbitrap-MS analysis provided a fast separation of selected analytes within 14 min, thus demonstrating a high throughput processing of samples. The developed methodology was tested by intralaboratory validation in terms of recovery, repeatability, linear calibration ranges, instrumental and method limits of quantitation (i-LOQ and m-LOQ), and where possible, trueness was verified by analysis of certified reference materials (CRMs). Recoveries of analytes were between 80 and 119%, while the repeatability in terms of relative standard deviations (RSDs) was in the range from 1.2 to 15.5%. The measured values for both analyzed CRMs agreed with the provided consensus values, revealing the recovery of reference concentrations in 72-119% range. The elaborated method met the sensitivity criterion according to Commission Recommendation 2014/118/EU on monitoring of BFRs in food products for majority of the compounds. The concentrations of polybrominated diphenyl ethers (PBDEs) in real samples determined by HPLC-APPI-Orbitrap-MS method and validated gas chromatography-high-resolution mass spectrometry (GC-HRMS) method were found to be in a good agreement. CI - Copyright (c) 2015 Elsevier B.V. All rights reserved. FAU - Zacs, D AU - Zacs D AD - Institute of Food Safety, Animal Health and Environment "BIOR", Lejupes iela 3, Riga, LV-1076, Latvia. Electronic address: dzintars.zachs@gmail.com. FAU - Bartkevics, V AU - Bartkevics V AD - Institute of Food Safety, Animal Health and Environment "BIOR", Lejupes iela 3, Riga, LV-1076, Latvia; University of Latvia, Department of Chemistry, Kr. Valdemara iela 48, Riga, LV-1013, Latvia. LA - eng PT - Journal Article DEP - 20151020 PL - Netherlands TA - Anal Chim Acta JT - Analytica chimica acta JID - 0370534 OTO - NOTNLM OT - Atmospheric pressure photoionization OT - Brominated flame retardants OT - Liquid chromatography OT - Orbitrap mass spectrometry EDAT- 2015/11/04 06:00 MHDA- 2015/11/04 06:01 CRDT- 2015/11/04 06:00 PHST- 2015/06/22 00:00 [received] PHST- 2015/09/22 00:00 [revised] PHST- 2015/10/05 00:00 [accepted] PHST- 2015/11/04 06:00 [entrez] PHST- 2015/11/04 06:00 [pubmed] PHST- 2015/11/04 06:01 [medline] AID - S0003-2670(15)01242-8 [pii] AID - 10.1016/j.aca.2015.10.008 [doi] PST - ppublish SO - Anal Chim Acta. 2015 Oct 22;898:60-72. doi: 10.1016/j.aca.2015.10.008. Epub 2015 Oct 20.