Development of a new method for the enantiomer specific determination of HBCD using an ion trap mass spectrometer |
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Authors: | Gómara Belén Lebrón-Aguilar Rosa Quintanilla-López Jesús Eduardo González María José |
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Affiliation: | a Department of Instrumental Analysis and Environmental Chemistry, Institute of General Organic Chemistry (CSIC), Juan de la Cierva 3, 28006 Madrid, Spain b Institute of Physical Chemistry “Rocasolano” (CSIC), Serrano 119, 28006 Madrid, Spain c Departamento de Ingeniería Química Industrial y del Medio Ambiente, ETSI Industriales (UPM), José Gutiérrez Abascal 2, 28006 Madrid, Spain |
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Abstract: | An alternative method for the enantiomer specific determination of hexabromocyclododecanes (HBCD) by LC-ESI-MS/MS using an ion trap analyser is proposed. The method is based on the formation of a chlorine adduct (m/z 676.6) of the (±)α-, (±)β-, and (±)γ-HBCD enantiomers and their further fragmentation into their stable quasi-molecular ion (m/z 640.6). In this way, problems related to the ion trap low mass cutoff and variable amounts of other adduct peaks in the samples are solved. Parameters affecting separation, ionisation and MS/MS detection were studied. Method performance was also evaluated: calibration curves were found linear from 20 to 400 pg μL−1 for each enantiomer; detection limits ranged between 1.5 and 4.3 pg μL−1; repeatability and reproducibility, expressed as relative standard deviation, were lower than 6% and 13%, respectively. The application to different types of spiked samples (pork meat, lean fish, and butter) pointed out the occurrence of matrix effects that could be solved by using labelled standards. |
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Keywords: | Hexabromocyclododecane Liquid chromatography Tandem mass spectrometry Enantioselective method |
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