Revista de cromatografía y técnicas de separación

Revista de cromatografía y técnicas de separación
Acceso abierto

ISSN: 2157-7064


Análisis LC-MS de compuestos de carbonilo de bajo peso molecular como 2,4-dinitrofenilhidrazonas utilizando espectrometría de masas de ionización por aspersión electrónica en modo de iones negativos

Dag Ekeberg, Hans Ragnar Norli, Camilla Stene, Hanne Devle y Linda Bergaust

The accumulation of brominated fl ame retardants (BFRs) in the environment raises concern in light of observed detrimental effects on wildlife as well as on public health. We here present a recently modi fi ed method for the identi fi cation and quanti fi cation of the following selection of bromodiphenyl ether (BDE) fl ame retardants: BDE-17, -47, -66, -100, -153 and -183, in soil and sediments, using a new extraction procedure followed by gas chromatography mass spectrometry (GC-MS). Low- and high- resolution mass spectrometry (LRMS and HRMS, respectively) were compared and the latter was found to be superior with respect to both sensitivity and linear range. At LRMS mode the linear range was 3.8 – 19.2 ng/g dry weight (dw), while the use of HRMS more than doubled the linear range to 1.9 – 38.4 ng/g dry weight. Both methods were tested with regards to matrix associated effects on the limit of detection and quantitation. The use of HRMS yielded equal sensitivity for standards in solution and matrix. This was not the case when using LRMS. Here the limits of detection and quantitation were severely elevated by the matrix. Recoveries were comparable, but slightly higher at LRMS mode (77.0 – 121.9%) compared to HRMS (83.2 – 115.3%). The method described here is high throughput, low cost and will prove valuable in monitoring the levels of BFRs in the environment.