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Distribution and Fate of HBCD and TBBPA Brominated Flame Retardants in North Sea Estuaries and Aquatic Food Webs
Distribution and Fate of HBCD and
TBBPA Brominated Flame Retardants
in North Sea Estuaries and Aquatic
Food Webs
S T E V E N M O R R I S
Centre for Environment, Fisheries and Aquaculture Science,
Weymouth Laboratory, Barrack Road,
Weymouth, Dorset, United Kingdom DT4 8UB
C O L I N R . A L L C H I N
Centre for Environment, Fisheries and Aquaculture Science,
Burnham Laboratory, Remembrance Avenue,
Burnham-on-Crouch, Essex, United Kingdom CM0 8HA
B A R T N . Z E G E R S ,
J O R I S J . H . H A F T K A , A N D J A N P . B O O N
Royal Netherlands Institute for Sea Research, P. O. Box 59,
1790 AB Den Burg, Texel, The Netherlands
C L A U D E B E L P A I R E
Institute of Forestry and Game Management, Duboislaan 14,
B-1560 Hoeilaart, Belgium
P I M E . G . L E O N A R D S ,
S T E F A N P . J . V A N L E E U W E N , A N D
J A C O B D E B O E R *
Wageningen UR, Animal Sciences Group, Netherlands
Institute for Fisheries Research, P. O. Box 68,
1970 AB IJmuiden, The Netherlands
Tetrabromobisphenol A (TBBPA) and hexabromocy-
clododecane diastereoisomers (R-, -, and -HBCD) were
investigated in effluents from sewage treatment works,
landfill leachates, sediments, and food web organisms of
the North Sea basin. Residues were quantified by liquid
chromatography-mass spectrometry. Both flame retardants
were enriched in sewage sludges, where a maximum
total () HBCD concentration of 9.1 mg/kg (dry weight; d.w.)
was found; TBBPA was at levels of 10
2
µg/kg. Landfill
leachates from The Netherlands showed up to 36 mg (HBCD)/
kg (d.w.). -HBCD dominated isomeric profiles in sediments,
and concentrations were elevated near to a site of
HBCD manufacture. R-HBCD was the primary congener
detected in marine mammals; however, very few samples
exhibited TBBPA. HBCD ranged from 2.1 to 6.8 mg/kg
(lipid weight; l.w.) in liver and blubber of harbor porpoises
(
Phocoena phocoena) and seals (Phoca vitulina). TBBPA
levels in cormorant (
Phalacrocorax carbo) livers were up to
1 order of magnitude lower compared to HBCD. HBCD
in eels (
Anguilla anguilla) from the Scheldt basin (Belgium)
reflected the spatial distribution of concentrations in
local sediments. This study shows evidence of HBCD
bioaccumulation at the trophic level and biomagnification
in the ascending aquatic food chain, and these findings
justify risk assessment studies at the ecosystem level.
Introduction
Brominated flame retardants (BFRs) are comprised of several
different, high production volume chemicals that are used
to inhibit or impede flammability in combustible products
(1). Hexabromocyclododecane (HBCD, Figure 1) and tetra-
bromobisphenol A (TBBPA, Figure 2) are two BFRs currently
in use. HBCDs main application is to flame retard extruded
and expanded polystyrene that is used as thermal insulation
in buildings. A minor application for HBCD is in upholstery
textiles. The HBCD technical product is composed of three
diasteroisomers (R, , and ), with -HBCD contributing to
approximately 80% of technical formulation (2). TBBPA is
the primary flame retardant used in electronic circuit boards
and is covalently bound to the resin (2). Decabromodiphenyl
ether (deca-BDE) and TBBPA account for approximately 50%
of the worlds usage of BFRs. TBBPA is the most widely used
BFR and in 1999, 13 800 tonnes (t) of TBBPA and 8900 t of
HBCD were consumed in the European Union (EU) (3). The
usage of BFRs appears to differ among the countries or regions
of the world (4).
The widespread, environmental distribution of lower BDEs
is well-known, and publications have focused on that class
of BFRs (see ref 5 for review). Few studies report the presence
of HBCD and TBBPA in the environment. For example, HBCD
has been detected in indoor dust (6), and TBBPA has been
found in the interior of television sets (7). TBBPA has also
been reported in sludge collected from sewage treatment
works (STWs) and at concentrations up to 50 µg/kg (dry
weight; d.w.) (8, 9). The levels of HBCD, TBBPA, and BDEs
in river sediments sampled in the vicinity of Swedish textile
plants and a plastics industry applying these BFRs were higher
compared to concentrations upstream of discharge points
(10, 11). TBBPA has also been reported in sediment (12).
Tissues from mussels acquired downstream of a BFR
production facility in The Netherlands showed HBCD
concentrations up to 51 µg/kg (lipid weight; l.w.) (13). A mean
concentration of 124 µg(HBCD)/kg (l.w.) was found in
Guillemot eggs from the Baltic Proper (14), and temporal
trends studies of residue levels indicated a significant increase
from 1969 to 1997 (15). After 1997, an EU risk assessment
evaluated this study and concluded that the trend was leveling
off. HBCD has also been reported in arctic air and biota (16).
Although the evidence for the environmental presence of
HBCD and TBBPA is small, their detection in a wide range
of matrices alerts us to a potential environmental concern.
Previously published HBCD concentration data have been
derived by gas chromatography (GC) with either negative
ion chemical ionization mass spectrometry or GC with
electron capture detection (17). Analysis by GC has limitations
as the three diastereomers cannot be resolved chromato-
graphically (2), and they are thermally labile (18) at tem-
peratures (>160
°
C) that are commonly applied during GC
separation. Thus, HBCD values have been reported as total
() HBCD, although visible chromatographic peak broaden-
ing caused by thermal instability has resulted in less accurate
data. Through the application of liquid chromatography mass
spectrometry (LC-MS), it is now possible to separate R-, -,
and -HBCD diastereomers (19-21). To the best of our
knowledge, this is the first study to deploy LC-MS for the
simultaneous detection and quantification of the individual
HBCD diastereomers, and TBBPA in an extensive range
* Corresponding author phone: 31 (0) 255 564736; fax: 31 (0) 255
564644; e-mail: jacob.deboer@wur.nl.
10.1021/es049640i CCC: $27.50
©
xxxx American Chemical Society
VOL. xx, NO. xx, xxxx / ENVIRON. SCI. & TECHNOL.
9
A
PAGE EST: 7.1
Published on Web 00/00/0000 of biotic and abiotic compartments from the aqueous
environment. The identification of possible sources of these
BFRs is also described here.
The purpose of this research was to examine the occur-
rence of HBCD diastereomers and TBBPA in effluents from
STWs and landfill leachates and to determine concentrations
and diastereomeric profiles in sediments from rivers and
estuaries surrounding the North Sea. A further purpose was
to investigate their bioaccumulation in organisms represent-
ing the different trophic levels of the North Sea food web.
Three laboratories undertook comparisons of the LC-MS
technique and concluded that harmonized methods were
sufficiently robust to perform this study (22).
Experimental Section
A sample location map of sediment and biotic taken from
the rivers and estuaries of the North and Irish Seas and Scheldt
basin is presented in Figure 3.
Sampling of Eels and Sediments in the Scheldt Basin
(Belgium). Yellow eels (Anguilla anguilla) were taken in 2000
and from 16 locations in the Scheldt Basin and from three
reference sites (a: Warmebeek, Achel-kluis; b: Grote Bever-
dijk, Lo-Reninge; c: R. IJzer, Nieuwpoort). Either electro- or
fyke fishing techniques were used to collect the eels. At each
sampling location, tissue from 10 individual eels (30 to 50
cm length) were pooled prior to homogenization and analysis.
Samples of sediment were collected in August 2001 from the
same 19 locations with an additional sample taken at
Vrasenedoc in Beveren, Belgium. Ten sediment subsamples
were acquired at each site and by a van Veen grab, and these
were pooled and thoroughly homogenized prior to extraction.
Sample location details are given as Supporting Information
in Table SI-1.
Sediment and Food Web Samples from the Western
Scheldt, The Netherlands. In 2000, sediment samples from
19 locations in the Western Scheldt were acquired by a van
Veen grab (see Supporting Information Table SI-2). Sediment
samples from nine Dutch rivers (see Table SI-3) were also
taken during the same sampling period; yellow eels from the
same rivers had been collected in 1999 and by the methods
described above. At Terneuzen, eggs (n)10) from the
common tern (Sterna hirundo), one sample of mysid shrimp
(Crangon crangon), and one of sand goby (Pom