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1.
Environ Res ; 262(Pt 1): 119834, 2024 Aug 23.
Artigo em Inglês | MEDLINE | ID: mdl-39182753

RESUMO

A human biomonitoring study was conducted to assess the exposure of Hungarian children aged 8-11 years to ten phthalate esters (PEs) and DINCH between 2017 and 2018. In addition to collecting urine samples from 262 participants, a questionnaire was completed by the parents or legal guardians to identify potential determinants of exposure. The highest geometric mean concentration was observed for MiBP, followed by MBP, cx- MEHP, OH-MEHP and MEP. Three out of the four DINCH metabolites were detected in more than 90% of the samples. The comparison of the urinary concentrations measured in this study with those observed in the DEMOCOPHES study revealed a significant decreasing trend in all PE metabolites investigated in both studies between 2011/2012 and 2017/2018. Different approaches were used to assess the health risks associated with the exposure to PEs and DINCH. Our results highlighted that the hazard index (HI) values were higher than 1 in 17.6% of the children when the human biomonitoring guidance values were applied. In contrast, less than 3% of the children had HI values exceeding 1 when other sources of reference values were used. By applying a safety factor of 10 for the risk assessment, 17.6-91.6% of the children were characterized by HI values higher than 0.1, indicating the need for risk reduction measures. Overall, DnBP, DiBP and DEHP were identified as the main drivers of the mixture risk. Although PEs and DINCH are ubiquitous contaminants, there are still inconsistencies and gaps in our understanding of the determinants of exposure. The results of the multivariate regression analysis showed significant associations between PE or DINCH metabolite concentrations and certain individual characteristics, use of personal care products, home and school environment and food and beverages consumption 24 h prior to sample collection.

2.
Inorg Chem ; 61(36): 14403-14418, 2022 Sep 12.
Artigo em Inglês | MEDLINE | ID: mdl-36044722

RESUMO

Research on new reaction routes and precursors to prepare catalysts for CO2 hydrogenation has enormous importance. Here, we report on the preparation of the permanganate salt of the urea-coordinated iron(III), [hexakis(urea-O)iron(III)]permanganate ([Fe(urea-O)6](MnO4)3) via an affordable synthesis route and preliminarily demonstrate the catalytic activity of its (Fe,Mn)Ox thermal decomposition products in CO2 hydrogenation. [Fe(urea-O)6](MnO4)3 contains O-coordinated urea ligands in octahedral propeller-like arrangement around the Fe3+ cation. There are extended hydrogen bond interactions between the permanganate ions and the hydrogen atoms of the urea ligands. These hydrogen bonds serve as reaction centers and have unique roles in the solid-phase quasi-intramolecular redox reaction of the urea ligand and the permanganate anion below the temperature of ligand loss of the complex cation. The decomposition mechanism of the urea ligand (ammonia elimination with the formation of isocyanuric acid and biuret) has been clarified. In an inert atmosphere, the final thermal decomposition product was manganese-containing wuestite, (Fe,Mn)O, at 800 °C, whereas in ambient air, two types of bixbyite (Fe,Mn)2O3 as well as jacobsite (Fe,Mn)T-4(Fe,Mn)OC-62O4), with overall Fe to Mn stoichiometry of 1:3, were formed. These final products were obtained regardless of the different atmospheres applied during thermal treatments up to 350 °C. Disordered bixbyite formed first with inhomogeneous Fe and Mn distribution and double-size supercell and then transformed gradually into common bixbyite with regular structure (and with 1:3 Fe to Mn ratio) upon increasing the temperature and heating time. The (Fe,Mn)Ox intermediates formed under various conditions showed catalytic effect in the CO2 hydrogenation reaction with <57.6% CO2 conversions and <39.3% hydrocarbon yields. As a mild solid-phase oxidant, hexakis(urea-O)iron(III) permanganate, was found to be selective in the transformation of (un)substituted benzylic alcohols into benzaldehydes and benzonitriles.

3.
Angew Chem Int Ed Engl ; 61(37): e202208420, 2022 Sep 12.
Artigo em Inglês | MEDLINE | ID: mdl-35876269

RESUMO

[1,2]-shift of atoms in alkyl fragments belongs to the class of dyotropic rearrangements. Various atoms, including halogens can be involved in the migration, however participation of iodine is unprecedented. Herein, we report our experimental and DFT studies on the oxidation triggered dyotropic rearrangement of iodo and chloro functions via butterfly-type transition state to demonstrate the migrating ability of λ3 -iodane centre. With the exploitation of dyotropic rearrangement we designed and synthesized a novel fluoroalkyl iodonium reagent from industrial feedstock gas HFO-1234yf. We demonstrated that the hypervalent reagent serves as an excellent fluoroalkylation agent for various amines and nitrogen heterocycles.

4.
Sci Rep ; 11(1): 8951, 2021 04 26.
Artigo em Inglês | MEDLINE | ID: mdl-33903673

RESUMO

The use of cannabidiol (CBD) in electronic cigarettes is widespread. Previously, it was reported that CBD is partly transformed to THC in case smoking as a cigarette, however, the pyrolysis of this compound has not been assessed extensively. The aim of our study was to investigate the effect of temperature on the composition of pyrolysis products of CBD. The experiments were performed in the typical operating temperature range of e-cigarettes (250-400 °C) and at 500 °C under both inert and oxidative conditions, and the pyrolysis products were identified and quantified by GC-MS. Depending on the temperature and atmosphere, 25-52% of CBD was transformed into other chemical substances: Δ9-THC, Δ8-THC, cannabinol and cannabichromene were the predominant pyrolysates in both conditions, all formed by cyclization reaction. THC was the main pyrolysis product at all temperatures under both oxidative and inert conditions. Our results point out that CBD in e-cigarettes can be considered as a precursor of THC, thus it bears all the dangers related to this psychoactive compound. Our findings are fundamental contributions to the safety profile of CBD-based e-cigarettes.


Assuntos
Canabidiol/química , Canabinoides , Dronabinol , Sistemas Eletrônicos de Liberação de Nicotina , Canabinoides/análise , Canabinoides/química , Dronabinol/análise , Dronabinol/química , Pirólise
5.
Biosci Biotechnol Biochem ; 73(1): 93-103, 2009 Jan.
Artigo em Inglês | MEDLINE | ID: mdl-19129649

RESUMO

Chitin is an insoluble component in the shells of several molluscan species. It is thought to play important roles, in biomineralization and shell structure. To date, however, reports are scarce and sometimes contradictory, and suffer from methodological problems. Only in a single cephalopod species has the chitin been identified as beta-chitin. We present data on chitin occurrence in 22 species of shell-bearing Mollusca (Conchifera) and Polyplacophora, including the first evidence for scaphopods, based on pyrolysis gas chromatography, mass spectrometry (GC-MS), and infrared spectroscopy (IR). Pyrolysis GC-MS detected chitin in every tested member of the Conchifera. IR spectroscopy before and after chitinase treatment revealed at least three distinct patterns of peak changes. The contents of the insoluble shell organics included not only chitin and proteins, but also insoluble polysaccharides, e.g., glucan. We conclude that chitin was present in the last common ancestor of the Conchifera and that its abundance in the shell matrix depends on the differentiation of the shell.


Assuntos
Quitina/análise , Moluscos , Animais , Evolução Biológica , Cromatografia Gasosa-Espectrometria de Massas/métodos , Polissacarídeos/análise , Proteínas/análise , Espectrofotometria Infravermelho/métodos
6.
Sci Total Environ ; 458-460: 451-8, 2013 Aug 01.
Artigo em Inglês | MEDLINE | ID: mdl-23688967

RESUMO

Carbonated and non-carbonated mineral water samples bottled in 0.5-L, 1.5-L and 2.0-L polyethylene terephthalate (PET) containers belonging to three different water brands commercialized in Hungary were studied in order to determine their phthalate content by gas chromatography-mass spectrometry. Among the six investigated phthalates, diisobutyl phthalate, di-n-butyl-phthalate, benzyl-butyl phthalate and di(2-ethyl-hexyl) phthalate (DEHP) were determined in non-carbonated samples as follows: <3.0 ng L(-1)-0.2 µg L(-1), <6.6 ng L(-1)-0.8 µg L(-1), <6.0 ng L(-1)-0.1 µg L(-1) and <16.0 ng L(-1)-1.7 µg L(-1), respectively. Any of the above-mentioned phthalate esters could be detected in carbonated mineral water samples. DEHP was the most abundant phthalate in the investigated samples. It could be detected after 44 days of storage at 22 °C and its leaching was the most pronounced when samples were stored over 1200 days. Mineral water purchased in PET bottles of 0.5L had the highest phthalate concentrations compared to those obtained for waters of the identical brand bottled in 1.5-L or 2.0-L PET containers due to the higher surface/volume ratio. No clear trend could be established for phthalate leaching when water samples were kept at higher temperatures (max. 60 °C) showing improper storage conditions. Phthalate determination by pyrolysis-gas chromatography/mass spectrometric measurements in the plastic material as well as in the aqueous phase proved the importance of the quality of PET raw material used for the production of the pre-form (virgin vs. polymer containing recycled PET).


Assuntos
Água Carbonatada/análise , Água Potável/química , Águas Minerais/análise , Ácidos Ftálicos/análise , Polietilenotereftalatos/química , Dibutilftalato/análogos & derivados , Dietilexilftalato , Cromatografia Gasosa-Espectrometria de Massas , Hungria , Temperatura
7.
J Chromatogr A ; 1130(1): 91-6, 2006 Oct 13.
Artigo em Inglês | MEDLINE | ID: mdl-16750213

RESUMO

The capability of solid porous catalysts has been studied for the destruction or modification of halogenated aromatic compounds contaminating the pyrolysis oil of recycled plastics from electronic waste. A fast and simple experimental procedure is carried out using a micropyrolyser coupled to GC-MS in such a way that catalyst microbed was placed in the sample tube of the pyrolyser. The pyrolysis products of polycarbonate blended with a frequently applied flame retardant tetrabromobisphenol A (TBBPA) and epoxy resin containing TBBPA monomer units have been analysed, and the brominated components were compared with the thermal decomposition products of TBBPA and its diallyl ether. When TBBPA vapour passes through molecular sieve 4A a slight debromination and a partial cleavage of bisphenol A into phenols occur. Over molecular sieves of larger pore size (13X and NaY zeolite) an important decrease of TBBPA amount is observed indicating effective trapping ability of these catalysts of basic character for brominated aromatic compounds. A total chemical modification of the vapour was achieved by Al-MCM-41 catalyst that split TBBPA into bromophenols. Analogous results were obtained by carrying out similar experiments on diallyl ether of TBBPA. Moreover, it was revealed that brominated bisphenol A compounds are modified essentially the same way, either evaporated or evolved from a polycarbonate blend or produced by pyrolysis from an epoxy resin.


Assuntos
Catálise , Cromatografia Gasosa-Espectrometria de Massas/métodos , Bifenil Polibromatos/química , Resinas Epóxi/química , Retardadores de Chama/análise , Cromatografia Gasosa-Espectrometria de Massas/instrumentação , Halogenação , Cimento de Policarboxilato/química
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