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Técnica: LCMS. Orbitrap. Preparación de muestras.

Área de trabajo: Medio Ambiente. Regulaciones y Normativas.

Título: Desarrollo de Método para la Determinación de Nuevos Retardantes de llama Bromados, usando un Espectrómetro de Masa Q Exactive HRAM.

Título original: Method Development for the Identification of Novel Brominated Flame Retardants Using a Q Exactive HRAM Mass Spectrometer

Autor: Zoltan Szabo1, Junhua Wang2, Yury Agroskin1, Jim Thayer1, Julian Saba2,3, Rosa Viner2, Andreas Huhmer2, Jeff Rohrer1, Liu Yan1, Kannan Srinivasan1, Dietmar Reusch4, and Christopher A. Pohl 11 Thermo Fisher Scientific, Sunnyvale, CA, USA; 2Thermo Fisher Scientific, San Jose, CA, USA; 3Thermo Fisher Scientific, Mississauga, ON, Canada; 4Roche Diagnostics GmbH, Penzberg, Germany.




Purpose: Identification of legacy and novel brominated flame retardants in dust samples on Thermo Scientific™ Quadrupole-Orbitrap™ benchtop instrumentation.

Methods: Identification and screening of brominated substances of interest was conducted in dust samples.

Results: Dust might be a relevant source of brominated flame retardants and therefore interesting for human exposure. HRAM instrumentation aids in the identification of these compounds.


Due to legislative restrictions on manufacture and use of some brominated flame retardants (BFRs), several new chemicals (NBFRs) have been developed. To explore their presence in different environmental compartments and ultimately understand their environmental fate, analytical methods for targeted analysis are required [1]. Classically these compounds are determined by GC-based instrumental methods. In recent years, LC-based methods coupled to low resolution mass spectrometers have also been developed [2]. Advances in high resolution mass spectrometry facilitate accurate measurements and identification of unknowns, including degradation and transformation products. Moreover, bromine isotopic pattern analysis as well as the use of mass defect plots and filters, helps identify relevant substances, with such techniques starting to be more commonly used in environmental science [3].


Sample Preparation 0.5 g of dust was weighed, spiked with mass-labeled TBBP-A and mixed with diatomaceous earth as dispersant. Extraction was conducted using a Thermo Scientific™ Dionex™ ASE™ 350 accelerated solvent extractor and in-cell cleanup (Figure 1). Chemical adsorbents silica and Florisil™ were employed to reduce possible matrix interferences. Extraction solvents included hexane, dichloromethane and acetone. Samples were evaporated to dryness using a Thermo Scientific™ Rocket™ Evaporator system and then reconstituted in 2 mL of methanol:toluene (1:1). The extraction instrumentation is shown in Figure 2. Liquid Chromatography Final extracts were separated on a Thermo Scientific™ Accucore™


One mass scale applicable to environmental analytical chemistry is defined by the substitution of a hydrogen atom by a chlorine atom (H/Cl). In analogy to the Kendrick mass calculation, the conversion used here is based on the multiplication of each peak of a chosen mass spectrum by 34/33.96102 and plotting the nominal mass vs. the transformed mass defect.

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