PMID- 28593369 OWN - NLM STAT- MEDLINE DCOM- 20180409 LR - 20191210 IS - 1618-2650 (Electronic) IS - 1618-2642 (Linking) VI - 409 IP - 20 DP - 2017 Aug TI - Miniaturised sample preparation method for the multiresidual determination of regulated organohalogenated pollutants and related compounds in wild bird eggs. PG - 4905-4913 LID - 10.1007/s00216-017-0432-5 [doi] AB - A simplified, miniaturised matrix solid-phase dispersion (MSPD)-based method allowing the simultaneous extraction and purification of contaminants belonging to selected families of regulated persistent organic pollutants (POPs), i.e. polychlorinated biphenyls (PCBs), organochlorine pesticides (OCPs) and penta- to octa-polybrominated diphenyl ethers (PBDEs), and related contaminants of emerging concern, such as deca-BDE and Dechlorane Plus (DP), has been proposed. Wild bird eggs were used as biotic fat-containing model matrices. Once optimised, the procedure allowed sample preparation to be accomplished within 30 min, in a single step, and with minimal sample and reagent consumption and waste generation. These features contributed to speeding up and greening the analytical process as compared to the large-scale multistep procedures for these types of analyses. The method was combined with gas chromatography-quadrupole mass spectrometry (GC-qMS) for PCB and OCP analysis and with GC-negative ion chemical ionisation-quadrupole mass spectrometry (NCI-qMS) for PBDE and DP determination. The complete analytical method provided satisfactory recoveries of the target compounds (above 83% for all analytes, except for PBDE 209, 63%), although as small an amount of sample as 0.300 g was used. The repeatability of the complete procedure was less than 16% (with the only exception for PCB 153, which looked to be affected by an interference). The limits of detection were in all cases lower than 34 pg g(-1) dry weight (as calculated for real samples), demonstrating the feasibility of the proposed procedure for accurate determination of the target compounds in biological samples. The proposed procedure was applied to the analysis of the target POPs in unhatched eggs of wild bird species. Graphical abstract Scheme of the miniaturised methodology proposed for environmental monitoring of POPs and related compounds in wild bird eggs. FAU - Roscales, Jose L AU - Roscales JL AD - Department of Instrumental Analysis and Environmental Chemistry, Institute of Organic Chemistry, CSIC (IQOG-CSIC), Juan de la Cierva 3, 28006, Madrid, Spain. FAU - Vicente, Alba AU - Vicente A AD - Department of Instrumental Analysis and Environmental Chemistry, Institute of Organic Chemistry, CSIC (IQOG-CSIC), Juan de la Cierva 3, 28006, Madrid, Spain. FAU - Ramos, Lourdes AU - Ramos L AD - Department of Instrumental Analysis and Environmental Chemistry, Institute of Organic Chemistry, CSIC (IQOG-CSIC), Juan de la Cierva 3, 28006, Madrid, Spain. l.ramos@iqog.csic.es. FAU - Jimenez, Begona AU - Jimenez B AD - Department of Instrumental Analysis and Environmental Chemistry, Institute of Organic Chemistry, CSIC (IQOG-CSIC), Juan de la Cierva 3, 28006, Madrid, Spain. LA - eng PT - Journal Article PT - Validation Study DEP - 20170607 PL - Germany TA - Anal Bioanal Chem JT - Analytical and bioanalytical chemistry JID - 101134327 RN - 0 (Environmental Pollutants) RN - 0 (Halogens) SB - IM MH - Animals MH - Birds MH - Eggs/*analysis MH - Environmental Pollutants/*analysis MH - Halogens/*analysis MH - Limit of Detection MH - *Miniaturization MH - Quality Control MH - Reproducibility of Results OTO - NOTNLM OT - DPs OT - MSPD OT - Miniaturisation OT - Multiresidual analysis OT - PBDEs OT - POPs EDAT- 2017/06/09 06:00 MHDA- 2018/04/10 06:00 CRDT- 2017/06/09 06:00 PHST- 2017/03/30 00:00 [received] PHST- 2017/05/24 00:00 [accepted] PHST- 2017/05/18 00:00 [revised] PHST- 2017/06/09 06:00 [pubmed] PHST- 2018/04/10 06:00 [medline] PHST- 2017/06/09 06:00 [entrez] AID - 10.1007/s00216-017-0432-5 [pii] AID - 10.1007/s00216-017-0432-5 [doi] PST - ppublish SO - Anal Bioanal Chem. 2017 Aug;409(20):4905-4913. doi: 10.1007/s00216-017-0432-5. Epub 2017 Jun 7.