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https://doi.org/10.37358/Rev.Chim.1949

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Revista de Chimie (Rev. Chim.), Year 2017, Volume 68, Issue 8, 1685-1689

https://doi.org/10.37358/RC.17.8.5744

Florentina Laura Chiriac, Liliana Cruceru, Marcela Niculescu, Luoana Florentina Pascu, Carol Blaziu Lehr, Toma Galaon

Simultaneous Determination of alfa-, beta- and gama-hexabromocyclododecane Diastereoisomers in Sewage Sludge using Liquid Chromatography Tandem Mass Spectrometry

Abstract:

Hexabromocyclododecane (HBCD) is a large-scale usage brominated flame retardant consisting of a mixture of diastereoisomers which has been reported as an ubiquitous environmental contaminant. HBCD has attracted much attention due to its toxicity and increasing levels in waste water sewage sludge. Since November 2014, HBCD was added to the Persistent Organic Pollutants list of the Stockholm Convention which generated a higher concern regarding its presence in the environment. A rapid (8 min) and accurate liquid chromatography electrospray ionization tandem mass spectrometry method (LC-ESI-MS/MS) was developed to separate and detect a-, b- and g-HBCD isomers from sewage sludge. Optimization of LC-MS parameters (column temperature, mobile phase composition and flow, collision energy, fragmentor voltage, capillary voltage and drying gas temperature) allowed complete separation of the three isomers and also very good detection sensitivity with instrumental quantitation limits (IQLs) between 0.3 and 0.6 ng/mL. The three isomers were separated on a C18 reversed-phase column, kept at 18°C, using a H2O/ACN/MeOH mobile phase mixture and detected by negative electrospray ionization using MRM mode with two transitions, one for quantitation and one for confirmation. MS detector response was linear in the range 1.0 ÷ 100.0 ng/mL with correlation coefficients (R2) higher than 0.99 for all three isomers. A simple ultrasonic assisted liquid-solid extraction procedure using a solvent mixture was employed to extract HBCD isomers from WWTP sewage sludge. Overall method intra-day and inter-day precision (RSD%) were situated between 7.6 ÷ 9.2% and 10.3 ÷ 14.5%, respectively. LOQs for a-, b- and g-HBCD were 1.4, 0.7 and 1.0 ng/g, comparable and even lower to those reported by similar studies concerning HBCD presence in WWTP sewage sludge. HBCD presence was tested from several WWTP sludge samples. All three isomers were found with 100% detection frequency ranging from 3 to 76 ng/g.
Keywords:
hexabromocyclododecane (HBCD); brominated flame retardants (BFRs); WWTP sewage sludge; ultrasonic assisted liquid-solid extraction; LC-MS/MS

Issue: 2017, Volume 68, Issue 8
Pages: 1685-1689
Publication date: 2017/9/15
https://doi.org/10.37358/RC.17.8.5744
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Creative Commons License
This article is published under the Creative Commons Attribution 4.0 International License
Citation Styles
Cite this article as:
CHIRIAC, F.L., CRUCERU, L., NICULESCU, M., PASCU, L.F., LEHR, C.B., GALAON, T., Simultaneous Determination of alfa-, beta- and gama-hexabromocyclododecane Diastereoisomers in Sewage Sludge using Liquid Chromatography Tandem Mass Spectrometry, Rev. Chim., 68(8), 2017, 1685-1689.

Vancouver
Chiriac FL, Cruceru L, Niculescu M, Pascu LF, Lehr CB, Galaon T. Simultaneous Determination of alfa-, beta- and gama-hexabromocyclododecane Diastereoisomers in Sewage Sludge using Liquid Chromatography Tandem Mass Spectrometry. Rev. Chim.[internet]. 2017 Aug;68(8):1685-1689. Available from: https://doi.org/10.37358/RC.17.8.5744


APA 6th edition
Chiriac, F.L., Cruceru, L., Niculescu, M., Pascu, L.F., Lehr, C.B. & Galaon, T. (2017). Simultaneous Determination of alfa-, beta- and gama-hexabromocyclododecane Diastereoisomers in Sewage Sludge using Liquid Chromatography Tandem Mass Spectrometry. Revista de Chimie, 68(8), 1685-1689. https://doi.org/10.37358/RC.17.8.5744


Harvard
Chiriac, F.L., Cruceru, L., Niculescu, M., Pascu, L.F., Lehr, C.B., Galaon, T. (2017). 'Simultaneous Determination of alfa-, beta- and gama-hexabromocyclododecane Diastereoisomers in Sewage Sludge using Liquid Chromatography Tandem Mass Spectrometry', Revista de Chimie, 68(8), pp. 1685-1689. https://doi.org/10.37358/RC.17.8.5744


IEEE
F.L. Chiriac, L. Cruceru, M. Niculescu, L.F. Pascu, C.B. Lehr, T. Galaon, "Simultaneous Determination of alfa-, beta- and gama-hexabromocyclododecane Diastereoisomers in Sewage Sludge using Liquid Chromatography Tandem Mass Spectrometry". Revista de Chimie, vol. 68, no. 8, pp. 1685-1689, 2017. [online]. https://doi.org/10.37358/RC.17.8.5744


Text
Florentina Laura Chiriac, Liliana Cruceru, Marcela Niculescu, Luoana Florentina Pascu, Carol Blaziu Lehr, Toma Galaon,
Simultaneous Determination of alfa-, beta- and gama-hexabromocyclododecane Diastereoisomers in Sewage Sludge using Liquid Chromatography Tandem Mass Spectrometry,
Revista de Chimie,
Volume 68, Issue 8,
2017,
Pages 1685-1689,
ISSN 2668-8212,
https://doi.org/10.37358/RC.17.8.5744.
(https://revistadechimie.ro/Articles.asp?ID=5744)
Keywords: hexabromocyclododecane (HBCD); brominated flame retardants (BFRs); WWTP sewage sludge; ultrasonic assisted liquid-solid extraction; LC-MS/MS


RIS
TY - JOUR
T1 - Simultaneous Determination of alfa-, beta- and gama-hexabromocyclododecane Diastereoisomers in Sewage Sludge using Liquid Chromatography Tandem Mass Spectrometry
A1 - Chiriac, Florentina Laura
A2 - Cruceru, Liliana
A3 - Niculescu, Marcela
A4 - Pascu, Luoana Florentina
A5 - Lehr, Carol Blaziu
A6 - Galaon, Toma
JF - Revista de Chimie
JO - Rev. Chim.
PB - Revista de Chimie SRL
SN - 2668-8212
Y1 - 2017
VL - 68
IS - 8
SP - 1685
EP - 1689
UR - https://doi.org/10.37358/RC.17.8.5744
KW - hexabromocyclododecane (HBCD)
KW - brominated flame retardants (BFRs)
KW - WWTP sewage sludge
KW - ultrasonic assisted liquid-solid extraction
KW - LC-MS/MS
ER -


BibTex
@article{RevCh2017P1685,
author = {Chiriac Florentina Laura and Cruceru Liliana and Niculescu Marcela and Pascu Luoana Florentina and Lehr Carol Blaziu and Galaon Toma},
title = {Simultaneous Determination of alfa-, beta- and gama-hexabromocyclododecane Diastereoisomers in Sewage Sludge using Liquid Chromatography Tandem Mass Spectrometry},
journal = {Revista de Chimie},
volume = {68},
number = {8},
pages = {1685-1689},
year = {2017},
issn = {2668-8212},
doi = {https://doi.org/10.37358/RC.17.8.5744},
url = {https://revistadechimie.ro/Articles.asp?ID=5744}
}
 
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