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Enantiomeric specific determination of hexabromocyclododecane by liquid chromatography–quadrupole linear ion trap mass spectrometry in sediment samples
|Authors:||Guerra, Paula ; Eljarrat, Ethel ; Barceló, Damià|
Liquid chromatography–quadrupole linear ion trap mass spectrometry (LC-QqLIT-MS)
|Citation:||Journal of Chromatography A 1203(1): 81-87 (2008)|
|Abstract:||This paper describes the determination and quantitation of hexabromocyclododecane (HBCD) enantiomers by liquid chromatography–quadrupole linear ion trap mass spectrometry (LC–QqLIT-MS). The method is based on the use of a chiral chromatographic column Nucleodex β-PM (200 mm × 4.0 mm, 5 μm), which allows a good separation between HBCD enantiomers [(±)α, (±)β and (±)γ] in less than 15 min and the detection is performed by a Q-Trap instrument. Linearity was checked between 0.05 and 25 injected ng. Limits of detection (LODs) were in the range of 0.3–1.5 pg, limits of quantification (LOQs) were between 1 and 6 pg, and both values are lower than those published in the literature applying LC–MS–MS methods. The method was applied to sediment samples collected along the Cinca River, a tributary of the Ebro River (northeast of Spain). Samples were extracted and purified following a pressurized liquid extraction method. LODs of the method were between 0.12 and 5.61 ng/g and LOQs, from 0.38 to 1.87 ng/g. Total HBCD levels in these sediments ranged from not detected to 2660 ng/g dry weight. Enantiomeric fractions (EFs) were calculated and compared with EF obtained from standard injections. It is important to note that calculated EFs were corrected using 2H18-labeled HBCD standards, in order to compensate matrix effect. EFs obtained in sediment samples suggested a higher presence of (+)α-HBCD and (+)γ-HBCD in technical mixture, this suggests that it is not a racemic mixture.|
|Description:||7 pages, 4 figures, 4 tables.-- PMID: 18656883 [PubMed].-- Printed version published Aug 29, 2008.|
Presented at the 4th International Workshop on Liquid Chromatography–Tandem Mass Spectrometry for Screening and Trace Level Quantitation in Environmental and Food Samples, Barcelona, Spain, 7–8 February 2008.
|Publisher version (URL):||http://dx.doi.org/10.1016/j.chroma.2008.07.027|
|Appears in Collections:||(IDAEA) Artículos|
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