0000000000180349

AUTHOR

Jekaterina Rjabova

The occurrence of Dechlorane Plus and related norbornene-based flame retardants in Baltic wild salmon (Salmo salar)

Twenty five Baltic wild salmon (Salmo salar) specimens were analysed for the content of Dechlorane-related compounds (DRCs). Out of the ten analysed DRCs, seven compounds were detected in the muscle tissues of salmon, including Dechlorane (Dec) 602, Dec 603, syn- and anti-stereoisomers of Dechlorane Plus (DP), Dechlorane Plus monoadduct (1,3-DPMA), hexachlorocyclopentadienyl-dibromocyclooctane (DBHCTD), and Mirex. The concentrations of Dec 604 and two DP dechlorinated compounds - decachloropentacyclooctadecadiene (Cl10DP) and undecachloropentacyclooctadecadiene (Cl11DP) - were below the limit of detection in all samples. The aggregated concentrations of DRCs (ΣDRC) were in the range of 551-…

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Ultra high performance liquid chromatography-time-of-flight high resolution mass spectrometry in the analysis of hexabromocyclododecane diastereomers: method development and comparative evaluation versus ultra high performance liquid chromatography coupled to Orbitrap high resolution mass spectrometry and triple quadrupole tandem mass spectrometry.

An efficient ultra high performance liquid chromatography (UHPLC)-time-of-flight high resolution mass spectrometry (TOF-HRMS) method was elaborated for the determination of hexabromocyclododecane (HBCD) diastereomers in fish samples and compared against UHPLC-Orbitrap-HRMS and UHPLC-triple quadrupole (QqQ) tandem MS (MS/MS) techniques. The TOF-HRMS analyzer was operated at high resolution (>10000 full width at half maximum (FWHM)) with scanning the m/z range from 600 to 700, to achieve picogram quantitation limits. The effects of various operational parameters on the instrumental response were systematically investigated. Evaluation of the influence of sample clean-up procedure steps on sig…

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The development and validation of a rapid method for the determination of antimicrobial agent residues in milk and meat using ultra performance liquid chromatography coupled to quadrupole – Orbitrap mass spectrometry

Abstract A new multi-class method has been developed for the identification and quantification of the residues of 26 antibiotics from different classes (sulfonamides, macrolides, tetracyclines, penicillins, and quinolones) in milk and meat by ultra performance liquid chromatography coupled to hybrid quadrupole – high resolution Orbitrap mass spectrometry (UPLC–qOrbitrap). The sample preparation included extraction of two analytical portions with acetonitrile and 5% trichloroacetic acid, respectively, followed by centrifugation and filtration. The method was validated over three days at 50% of MRL (maximum residue limit) set in the European Union. Experiments on spiked meat and milk samples …

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Occurrence of Brominated Persistent Organic Pollutants (PBDD/DFs, PXDD/DFs, and PBDEs) in Baltic Wild Salmon (Salmo salar) and Correlation with PCDD/DFs and PCBs

The contamination profiles of polybrominated dibenzo-p-dioxins (PBDDs), dibenzofurans (PBDFs), diphenyl ethers (PBDEs), and mixed monobromo/chloro dibenzo-p-dioxins (PXDDs) and dibenzofurans (PXDFs) were determined in the tissue of Baltic wild salmon and compared with those of polychlorinated dibenzo-p-dioxins (PCDDs), dibenzofurans (PCDFs), and biphenyls (PCBs). Out of the analyzed PXDD/DFs, only the 3-B-2,7,8-triCDF was detected (in the concentration range of 0.039-0.075 pg g(-1) fresh weight (f.w.)). The toxic equivalents (TEQs) for analyzed PBDD/DFs (0.074-0.142 pg TEQ g(-1) f.w.) were found to contribute on average 2.1% to the total PCDD/DF-PBDD/DF-TEQ. The total concentrations of 27 P…

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Development and optimization of gas chromatography coupled to high resolution mass spectrometry based method for the sensitive determination of Dechlorane plus and related norbornene-based flame retardants in food of animal origin

An analytical method has been developed for the trace determination of 10 dechlorane-related compounds (DRCs) in food products by gas chromatography - high resolution mass spectrometry (GC-HRMS). The highest sensitivity of this instrumental analysis method was achieved by selection of the GC column type, optimization of the heated zones within the instrument, and adjusting the electron impact energy. The efficiency of solid phase extraction as clean-up procedure was also optimized. Two different types of cartridges - neutral silica gel and Florisil®, as well as seven organic solvents or their mixtures - n-hexane, cyclohexane, acetone, toluene, n-hexane/ethyl acetate, n-hexane/acetone, and n…

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New perspectives on diastereoselective determination of hexabromocyclododecane traces in fish by ultra high performance liquid chromatography-high resolution orbitrap mass spectrometry.

a b s t r a c t A new analytical method is presented for diastereoisomer-specific identification and quantitation of hexabromocyclododecanes (HBCD) in fish samples. The method is based on extraction of the target analytes from samples with a mixture of organic solvents, with further three-stage clean-up includ- ing destructive removal of matrix components with sulphuric acid and acid-impregnated silica gel, and Florisil adsorption column chromatography. Ultra high performance liquid chromatography (UPLC) cou- pled with high resolution (HR) Orbitrap mass spectrometry featuring heated electrospray ionization (HESI-II) interface operated in negative ion mode was employed for the identification…

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Brominated flame retardants and toxic elements in the meat and liver of red deer (Cervus elaphus), wild boar (Sus scrofa), and moose (Alces alces) from Latvian wildlife.

In order to evaluate the contamination status of terrestrial biota in Latvia, muscle and liver tissues of red deer (Cervus elaphus), wild boar (Sus scrofa), and moose (Alces alces) were analyzed for the content of polybrominated diphenyl ethers (PBDE), hexabromocyclododecane (HBCD), tetrabromobisphenol A (TBBPA), as well as cadmium and lead. The highest mean concentrations of PBDEs (46.6pgg-1 wet weight (w.w.)), cadmium (0.95mgkg-1 w.w.), and lead (0.22mgkg-1 w.w.) were observed in the tissues of moose, while the wild boar samples contained the highest levels of HBCD, with the mean concentration equal to 264pgg-1 w.w. in muscle tissues. Generally low mean concentrations of TBBPA from 0.52 t…

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Brominated, chlorinated and mixed brominated/chlorinated persistent organic pollutants in European eels (Anquilla anquilla) from Latvian lakes

Fifty-eight European eel (Anquilla anquilla) specimens collected from five Latvian lakes were investigated for six groups of persistent organic pollutants (POPs), including polychlorinated, polybrominated and mixed bromo-chloro dibenzo-p-dioxins and dibenzofurans (PCDD/DFs, PBDD/DFs and PXDD/DFs), polychlorinated and mixed bromo-chloro biphenyls (PCBs and PXBs) and polybrominated diphenyl ethers (PBDEs). PCDD/DFs and PCBs were found to occur in the range 0.85–15.8 pg Total-WHO2005-TEQ g−1 f.w., and concentrations in most of the samples were below the maximum levels specified in European Commission Regulation (EU) No. 1259/2011. The summed concentrations of 27 PBDEs (∑PBDE) and 16 non-dioxin…

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Method development for the simultaneous determination of polybrominated, polychlorinated, mixed polybrominated/chlorinated dibenzo-p-dioxins and dibenzofurans, polychlorinated biphenyls and polybrominated diphenyl ethers in fish.

An analytical methodology was developed for simultaneous determination of five groups of persistent organic pollutants (POPs) including polybrominated, polychlorinated and mixed brominated-chlorinated dibenzo-p-dioxins and dibenzofurans (PBDD/DFs, PCDD/DFs and PXDD/DFs, respectively), polychlorinated biphenyls (PCBs) and polybrominated diphenyl ethers (PBDEs) in fish samples. The presented analytical approach was based on well established and robust method for determination of PCDD/DFs and PCBs, which was augmented with gas chromatography coupled to high resolution mass spectrometry (GC-HRMS) to include PBDEs, as well as poorly investigated PBDD/DFs and PXDD/DFs at toxicologically significa…

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