This study summarizes results on levels of 25 perfluoroalkyl substances (PFASs), three hexabromocyclododecane isomers (HBCDs), tetrabromobisphenol A (TBBPA), three brominated phenols and four hydroxylated derivates of polybrominated diphenyl ethers (OH-PBDEs) in 59fish samples collected in nine localities on two major rivers from the Czech Republic. To identify potential sources of these chemicals, several sampling sites located close to highly industrialized areas were also involved. The major PFAS representatives, perfluorooctane sulfonate (PFOS), C9-C14 perfluoroalkyl carboxylic acids (PFCAs) and perfluorooctane sulfonamide (FOSA) were detected in 100% fish samples. The concentration ranges of individual substances in the respective groups of PFASs were as follows: 0.572-61.3ngg(-)(1) wet weight (ww) for Tot-PFOS, 0.007-0.121ngg(-)(1)ww for perfluoroalkane sulfonates (PFSAs) (without PFOS isomers), 0.007-22.0ngg(-)(1)ww for PFCAs and 0.026-7.76ngg(-)(1)ww for FOSA. The highest contents of ∑PFASs (51.9ngg(-)(1)ww and 47.8ngg(-)(1)ww) were measured in fish muscle tissue from the locality Trmice situated on the Bílina River and Verdek on the Labe River, where chemical and/or textile industry is located. From 11 targeted BFRs, five compounds (α-HBCD, β-HBCD, γ-HBCD, TBBPA and 2,4,6-tribromophenol (TBP)) were determined in analyzed samples. The concentration ranged as follows: 3.15-1211ngg(-)(1) lipid weight (lw) for ∑HBCD, 4.99-203ngg(-)(1)lw for TBBPA and 1.76-107ngg(-)(1)lw for 2,4,6-TBP.
- MeSH
- chemické látky znečišťující vodu analýza MeSH
- fluorokarbony metabolismus MeSH
- halogenované uhlovodíky metabolismus MeSH
- monitorování životního prostředí * MeSH
- řeky chemie MeSH
- ryby metabolismus MeSH
- zvířata MeSH
- Check Tag
- zvířata MeSH
- Publikační typ
- časopisecké články MeSH
- práce podpořená grantem MeSH
- Geografické názvy
- Česká republika MeSH
Ultra-high-performance liquid chromatography coupled with quadrupole time-of-flight mass spectrometry (MS) and an alternative technology represented by direct analysis in real time coupled with quadrupole time-of-flight MS were investigated for metabolic fingerprinting of 343 red and white wine samples. Direct injection of pure wine and an extraction procedure optimized for isolation of polyphenols were used to compare different analytical and data handling strategies. After data processing and data pretreatment, principal component analysis was initially used to explore the data structure. Initially, the unsupervised models revealed a notable clustering according to the grape varieties, and therefore supervised orthogonal partial least squares discriminant analysis models were created and validated for separation of red and white wines according to the grape variety. The validated orthogonal partial least squares discriminant analysis models based on data (ions) recorded in positive ionization mode were able to classify correctly 95% of samples. In parallel, authentication parameters, such as origin and vintage, were evaluated, and they are discussed. A tentative identification of markers was performed using accurate mass measurement of MS and MS/MS spectra, different software packages and different online libraries. In this way, different flavonol glucosides and polyphenols were identified as wine markers according to the grape varieties.
A new method for rapid determination of 73 target organic environmental contaminants including 18 polychlorinated biphenyls, 16 organochlorinated pesticides, 14 brominated flame retardants and 25 polycyclic aromatic hydrocarbons in fish and fish feed using gas chromatography coupled with triple quadrupole tandem mass spectrometry (GC-MS/MS) was developed and validated. GC-MS/MS in electron ionization mode was shown to be a powerful tool for the (ultra)trace analysis of multiclass environmental contaminants in complex matrices, providing measurements with high selectivity and sensitivity. Another positive aspect characterizing the newly developed method is a substantial simplification of the sample preparation, which was achieved by an ethyl acetate QuEChERS (quick, easy, cheap, effective, rugged and safe) based extraction followed by silica minicolumn clean-up. With use of this sample preparation approach the sample laboratory throughput was increased not only because six samples may be prepared in approximately 1 h, but also because all the above-mentioned groups of contaminants can be determined in a single GC-MS/MS run. Under the optimized conditions, the recoveries of all target analytes in both matrices were within the range from 70 to 120% and the repeatabilities were 20% or less. The method quantification limits were in the range from 0.005 to 1 μg kg(-1) and from 0.05 to 10 μg kg(-1) for fish muscle tissue and fish feed, respectively. The developed method was successfully applied to the determination of halogenated persistent organic pollutants and polycyclic aromatic hydrocarbons in fish and fish feed samples.
- MeSH
- analýza hlavních komponent MeSH
- bezpečnost potravin metody MeSH
- kontaminace potravin MeSH
- krmivo pro zvířata normy MeSH
- látky znečišťující životní prostředí analýza chemie MeSH
- limita detekce MeSH
- plynová chromatografie s hmotnostně spektrometrickou detekcí * MeSH
- polycyklické aromatické uhlovodíky analýza normy MeSH
- řízení kvality MeSH
- ryby * MeSH
- tandemová hmotnostní spektrometrie * MeSH
- zvířata MeSH
- Check Tag
- zvířata MeSH
- Publikační typ
- časopisecké články MeSH
- práce podpořená grantem MeSH
The co-occurrence of deoxynivalenol-3-glucoside with its parent toxin, deoxynivalenol, has been recently documented in many cereal-based foods, especially in those produced by enzyme-catalyzed processes. The presence of this masked mycotoxin in the human diet has become an issue of health concern, mainly because of its assumed bioavailability. A selective immunoaffinity-based preconcentration strategy, followed by ultrahigh-performance liquid chromatography coupled with high-resolution orbitrap mass spectrometry, revealed that, in addition to the most common deoxynivalenol-3-glucoside, also oligoglycosylated deoxynivalenols with up to four bound hexose units were present in cereal-based products. The structure, origination, and fate of these deoxynivalenol conjugates during malt/beer production and bread baking have been thoroughly investigated. Special attention has been paid to the changes of deoxynivalenol conjugates enabled by industrial glycosidase-based enzymatic preparations. To the authors' best knowledge, this is the first study documenting the complexity of masked deoxynivalenol issue.
- MeSH
- chléb analýza MeSH
- Fusarium metabolismus MeSH
- glukosidy chemie MeSH
- jedlá semena chemie MeSH
- kontaminace potravin analýza MeSH
- molekulární struktura MeSH
- mykotoxiny chemie metabolismus MeSH
- pivo analýza MeSH
- trichotheceny chemie MeSH
- Publikační typ
- časopisecké články MeSH
- práce podpořená grantem MeSH
