Flame Retardants In Environmental Samples Research Articles

Development and validation of a liquid chromatography-mass spectrometry method for simultaneous analysis of triazine-based brominated flame retardants in environmental samples.

In the present study, a novel and reliable analytical method was developed and validated for the simultaneous determination of 1,3,5-tris(2,3-dibromopropyl)-1,3,5-triazine-2,4,6(1H,3H,5H)-trione (TDBP-TAZTO) and 2,4,6-tris(2,4,6-tribromophenoxy)-1,3,5-triazine (TTBP-TAZ) in environmental samples using high-performance liquid chromatography coupled to a tandem mass spectrometer. Firstly, for optimization of the liquid chromatography separation, mobile phases, oven temperatures, modifiers, and buffers were varied. Afterwards, the extraction efficiency of sediment and fish samples was tested with different techniques (pressurized liquid, solid-liquid, ultrasound-assisted, and Soxhlet extraction). Additionally, cleanup using modified multilayer silica gel (sediment) and gel permeation chromatography as well as Florisil® columns (fish) with several solvent mixtures were performed. The best results were obtained with the pressurized liquid extraction (optimal conditions: extraction solvent 100% toluene, extraction time 20min, cycles two, extraction temperature 100°C, and flushing volume 60%) compared to other solvent extraction methods. On the basis of this optimized analytical procedure, the method was validated with satisfactory values of correlation coefficient (R2) between 0.998 and 0.999 for both matrices in the calibration range of 2.0-502.0μgkg-1 for TDBP-TAZTO and 16.6-770.6μgkg-1 for TTBP-TAZ in sediment samples as well as 4.8-303.5μgkg-1 and 47.4-742.5μgkg-1 in fish samples (bream), respectively. Mean recoveries (n = 5) were calculated for both analytes with spiked matrices at one concentration level (100μgkg-1) between 98 and 114% with intra-day relative standard deviations less than 11%. The inter-day precision (n = 15) was also acceptable for both compounds < 11%. It was found that the limit of detection and limit of quantification were in the range of 0.4-1.3μgkg-1 for TDBP-TAZTO and 10-28μgkg-1 for TTBP-TAZ in surface sediment samples and 7-25μgkg-1 and 22-80μgkg-1 in fish samples (bream), respectively. The results indicated that these analytical methods could provide reliable and efficient approaches for quantification of TDBP-TAZTO and TTBP-TAZ in sediment and fish samples. Graphical abstract.

Correlated Raman micro-spectroscopy and scanning electron microscopy analyses of flame retardants in environmental samples: a micro-analytical tool for probing chemical composition, origin and spatial distribution

We present correlated application of two micro-analytical techniques: scanning electron microscopy/energy dispersive X-ray spectroscopy (SEM/EDS) and Raman micro-spectroscopy (RMS) for the non-invasive characterization and molecular identification of flame retardants (FRs) in environmental dusts and consumer products. The SEM/EDS-RMS technique offers correlated, morphological, molecular, spatial distribution and semi-quantitative elemental concentration information at the individual particle level with micrometer spatial resolution and minimal sample preparation. The presented methodology uses SEM/EDS analyses for rapid detection of particles containing FR specific elements as potential indicators of FR presence in a sample followed by correlated RMS analyses of the same particles for characterization of the FR sub-regions and surrounding matrices. The spatially resolved characterization enabled by this approach provides insights into the distributional heterogeneity as well as potential transfer and exposure mechanisms for FRs in the environment that is typically not available through traditional FR analysis. We have used this methodology to reveal a heterogeneous distribution of highly concentrated deca-BDE particles in environmental dust, sometimes in association with identifiable consumer materials. The observed coexistence of deca-BDE with consumer material in dust is strongly indicative of its release into the environment via weathering/abrasion of consumer products. Ingestion of such enriched FR particles in dust represents a potential for instantaneous exposure to high FR concentrations. Therefore, correlated SEM/RMS analysis offers a novel investigative tool for addressing an area of important environmental concern.

Novel combined stir bar sorptive extraction coupled with ultrasonic assisted extraction for the determination of brominated flame retardants in environmental samples using high performance liquid chromatography

A combined stir bar coated with poly (dimethysiloxane)-β-cyclodextrin (PDMS-β-CD) on single side has been prepared for the first time by sol–gel method and was coupled with ultrasonic assisted extraction (UAE) for the determination of some brominated flame-retardant compounds (BFRs) in soil and dust samples by high performance liquid chromatography (HPLC). Four different kinds of coatings including PDMS-β-CD, PDMS, carbowax (CW)-PDMS-poly (vinyl alcohol) (PVA) and PDMS-PVA were evaluated for stir bar sorptive extraction of BFRs by orthogonal experiment design. The experimental results reveal that the PDMS-β-CD combined stir bar exhibited the best extraction efficiency for the target analytes. The reproducibility for the preparation of PDMS-β-CD combined stir bar ranged from 1.3% to 15.7% in one batch, and 7.2% to 15.1% among batches. Extraction time, desorption solvent, concentration of methanol and NaCl in the matrix, pH, temperature and stirring speed were optimized. The combined stir bar can avoid direct friction of the coating with the bottom of the vessel, and could be used for more than 100 times. Linearity (>0.993), repeatability (<10.5%), reproducibility (<16.5%), recovery (56–118%) and detection limits (2.9–4.2 μg L −1) were proper to determine the seven BFRs. The developed method was applied to the determination of BFRs in soil and dust with satisfactory results.

Determination of Flame Retardants in Environmental Samples

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Determination of brominated flame retardants in environmental samples

The last few decades have seen dramatic growth in the scale of production and use of brominated flame retardants (BFRs). Not surprisingly, the levels of these compounds in the environment have increased as well. Even though the acute toxicity of most BFRs seems to be fairly low, some have shown similar toxic effects to PCBs and polychlorinated dibenzo- p-dioxins and furans. Thus, BFRs are a potential hazard to the environment and their levels in the environment must be monitored. This article gives a brief overview of the analytical methodology used for the determination of BFRs in environmental samples and the levels of BFRs found in the samples.