Chemosphere 90 (2013) 2467–2476

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Chemosphere
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Persistent organochlorine pesticide and PCB residues in surface sediments

of Lake Qarun, a protected area of Egypt
Assem O. Barakat a,⇑,1, Mohammed Khairy a,b,1, Inas Aukaily a,1
a
Department of Environmental Sciences, Faculty of Science, Alexandria University, Moharrem Bek, Alexandria 21511, Egypt
b
Graduate School of Oceanography, University of Rhode Island, 215 South Ferry Road, Narragansett, Rhode Island 02882, United States

h i g h l i g h t s

" High levels of OCs were found at sites near wastewater discharges.
" Ubiquitous contaminants were endrin, c-HCH, aldrin, CHLs, and endosulfan.
" The composition of DDT and its metabolites suggest old input of DDT.
" Levels of OCs were low to moderate compared to other locations worldwide.
" Areas of expected potential ecotoxicological risk were identified.

a r t i c l e i n f o a b s t r a c t

Article history: Organochlorine pesticides (OCPs) and polychlorinated biphenyls (PCBs) were determined in sediment
Received 8 July 2012 samples collected from 34 locations in Lake Qarun, Egypt to elucidate their concentrations, distribution,
Received in revised form 1 November 2012 possible sources and potential ecological risk. A total of 25 OCPs and 29 PCBs were identified and quan-
Accepted 4 November 2012
tified. OCPs and PCBs were found to be ubiquitous pollutants in the aquatic environment of Lake Qarun,
Available online 11 December 2012
particular near urban areas reflecting the local usage and input of these pollutants. Total concentrations
of OCPs and PCBs in sediments ranged from 1.01 to 164.8 ng g1 and 1.48 to 137.2 ng g1, respectively.
Keywords:
Among OCPs, c-HCH, heptachlor, aldrin, endrin, p,p0 -DDE, oxy-chlordane and endosulfan I and II were
Organochlorine pesticides
Metabolites
the most abundant compounds. The composition of PCB congeners was dominated by the tri-, tetra-,
Lake Qarun penta- and hexa-chlorinated biphenyls. The ratios of certain metabolites (isomers) to their parent
PCBs compounds (mixtures) indicated there are still new inputs of lindane, endrin, heptachlor and technical
P
Sediment endosulfan to Qarun Lake, while the ratios of (p,p0 -DDE + p,p0 -DDD)/ p,p0 -DDTs indicate earlier usage
of DDT. Contamination levels of PCBs and HCHs can be categorized as moderate to high compared to
other urbanized regions worldwide. According to established sediment quality guidelines, c-HCH, endrin
and chlordanes would be more concerned OCP species for the ecotoxicological risk in Lake Qarun.
Ó 2012 Elsevier Ltd. All rights reserved.

1. Introduction El-Shahawi et al., 2010). Because of their persistent, semivolatile

Persistent organic pollutants (POPs) such as organochlorine
pesticides (OCPs) and polychlorinated biphenyls (PCBs), are ubiq-
uitous pollutants in the environment that have caused worldwide
concern. For several decades, these compounds have been pro-
duced and extensively used world-wide for various applications
in industry and agriculture. Many organochlorines have been
implicated in a broad range of adverse human health and environ-
mental effects, including impaired reproduction, endocrine disrup-
tion, immuno suppression and cancer (Colborn et al., 1993;
⇑ Corresponding author. Tel.: +20 3 5463250; fax: +20 3 5463305.
E-mail address: asem.barakat@alex-sci.edu.eg (A.O. Barakat).
1
Fax: +20 3 3911794.
and bioaccumulative nature, long-range transport and biological
effects in the environment, they are restricted or banned globally
under the Stockholm Convention on Persistent Organic Pollutants
(Stockholm Convention, 2001, 2009).
Sediments act as a sink for POPs brought into the aquatic envi-
ronment from direct discharges, surface run-off and atmospheric
fall out. These and other chemicals may enter aquatic systems
through direct/indirect discharge, surface run-off and atmospheric
deposition. From such sinks, POPs and their residues can enter liv-
ing organisms, via flux through the water phase, and eventually
bioaccumulated in sediment-dwelling organisms and edible fish
(e.g., Licata et al., 2003; Chau, 2005). Therefore, the distribution
of POPs in sediments and biota can serve as a useful index of pol-
lution and potential environmental risks.

0045-6535/$ - see front matter Ó 2012 Elsevier Ltd. All rights reserved.
http://dx.doi.org/10.1016/j.chemosphere.2012.11.012
2468 A.O. Barakat et al. / Chemosphere 90 (2013) 2467–2476
With the rapid development of agriculture and industry in Egypt,
OCPs an PCBs and have been detected in various biotic and abiotic
environmental compartments (e.g., Barakat, 2003, 2004; El-Kady
et al., 2007; Mansour et al., 2009; Khairy et al., 2012; Barakat et al.,
2012a). In Egypt, uses of organochlorine pesticides began in the
1950s and were extensively used until 1981 to protect crops from in-
sects, disease fungi and weeds, to remove unwanted vegetation and
to control insects by the general public. The reported total active
ingredients of major organochlorine pesticides during a 30-year per-
iod are as follows: toxaphene 54,000 mt (1955–1961), endrin
10,500 mt (1961–1981), DDT 13,500 mt (1952–1971) and lindane
21,000 mt (1952–1978) (El-Sebae et al., 1993). The main use of these
organochlorine insecticides was the control of insects, specially the
cotton leafworm and bollworms in extensive agricultural produc-
tion. Based on the reports of their harmful effects to wildlife and hu-
mans, organochlorine pesticides were banned or restricted from use
or trade since 1988 and prohibited in Egypt by a Ministerial Decree
in 1996. However many of these contaminants have long environ-
mental half-lives, on the order of 10–20 years, and may continue
to be detected for many years (Jones and Voogt, 1999). Most studies
that examined the POPs in sediment were from marine and estuary
environment, and little information is available on POPs contamina-
tion in sediment from inland lakes in Egypt (Barakat, 2004).
Lake Qarun lies in the Faiyum Depression at the margin of the
Western Desert of Egypt, about 80 km to the southwest of Cairo,
and covers an area of 226 km2. It is an enclosed, saline, inland lake,
40 km in length, 5.7 km in width and 43 m below mean sea level. It
is a shallow lake with a mean depth of 4.2 m (Baioumy et al., 2011).
Lake Qarun is the third largest lake in Egypt and one of the oldest
lakes in the world. It is the existing remnant of the ancient prehis-
toric lake (Moeris Lake) that was over 75 m deep and covered more
than 2000 km2 of the Faiyum Depression (Shafei, 1960). It is rich in
both natural and archaeological resources because of the presence
of marine, fluvial and continental environment that goes back to
some 40 million years. The lake receives the agricultural and sew-
age drainage water from Faiyum Province and the neighboring cul-
tivated lands. Most of the drainage water reaches the lake through
two main drains, El-Batts at the northeastern corner and El-Wadi
near mid point of the southern shore, and two pump stations
(Fig. 1). Although Lake Qarun is designated as protected area in
Fig. 1. Study area and sampling sites in Lake Qarun, Egypt.
1989, the lake is suffering from serious water pollution problems
due to uncontrolled solid and liquid domestic and industrial waste
disposal practices, in addition to agrochemical contamination and
lack of sustainable wastewater management (Hussein et al.,
2008). Studies on the environmental health of Lake Qarun in Egypt
have concentrated in the past mostly on inorganic chemical analy-
sis of different ecosystem components (e.g., Saleh et al., 1988,
2000; Mansour and Sidky, 2003; Hussein et al., 2008). Data from
these studies showed that Lake Qarun is effected by pollution from
industrial and agricultural waste disposal. Except for a limited
study (Mansour and Sidky, 2003), which dealt with number of
OC pesticide residues in sediments from three locations from the
lake, no further information is yet available on the distribution
and sources of OCs in this important ecosystem. The objectives of
this work are to provide a survey of the concentration levels, distri-
butions and sources of PCBs and OCPs in surface sediment samples
from Lake Qarun and to assess their environmental risks in this ba-
sin. Compounds measured included 29 PCB congeners (PCB-8, 11,
18, 28, 44, 52, 66, 77, 81, 101, 105, 114, 118, 123, 126, 128, 138,
153 156, 157, 167, 169, 170, 180, 187, 189, 195, 206 and 209);
o,p0 -DDT, p,p0 -DDT and degradation products o,p0 -DDD, p,p0 -DDD,
o,p0 -DDE and p,p0 -DDE; chlordane related compounds (heptachlor
and its epoxide, oxy-, cis- and trans- chlordane, trans-nonachlor);
hexachlorobenzene (HCB); a-, b-, c-, and d-HCH; cyclodiene pesti-
cides (aldrin, dieldrin, endrin, endrin aldehyde, endrin ketone,
endosulfan I, II, and endosulfan sulphate) and methoxychlor. To
our knowledge, this is a first comprehensive study to report on
the concentrations of OCPs and PCBs in environmental samples
from Lake Qarun and provide baseline data for future research on
environmental occurrence and bioaccumulation of these com-
pounds in the study area.
2. Materials and methods
2.1. Study area and sampling
Thirty-four sites throughout the lake were sampled in January
2011 to analyze the contents of PCBs and OCPs in the surface sed-
iments. The sampling stations were selected as such to cover areas
 A.O. Barakat et al. / Chemosphere 90 (2013) 2467–2476
affected by agricultural and sewage drainage water from Faiyum
Province and the neighboring cultivated lands, and included the
outfalls of the El-Wadi and El-Batts drains and the two pumping
stations in the south and the southwest areas of the lake (Fig. 1).
Approximately top 0–5 cm of sediment was collected by a stainless
steel grab sampler. All the samples were stored in the pre-
combusted amber glass jar with Teflon lined lids and were stored
in the dark at 20 °C.
2.2. Analytical procedure
Sample preparation, extraction, and clean-up were performed
using a modification of the procedure of Wade et al. (2008). Briefly,
about 10 g freeze-dried sediment were soxhlet extracted with
methylene chloride for 48 h after spiking with 10 lL of a surrogate
standard mixture composed of carbon labeled pesticides and PCBs
(13C12 HCB, 13C12 p,p0 -DDT, 13C12 PCB 8, 28, 52, 118, 138, 180, 209;
5 ng lL1 in nonane). The solvent was concentrated in a rotary
evaporator to a final volume of 2 mL. During concentration of the
solvent, dichloromethane was exchanged for hexane. Extracts were
then fractionated by alumina:silica open column chromatography.
The column was slurry packed from the bottom to the top with 1 g
anhydrous sodium sulfate (previously baked at 400 °C for 4 h), 10 g
of 1% deactivated alumina (Brockman I, chromatographic grade,
combusted at 440 °C for 4 h and deactivated by adding the appro-
priate volume of Milli-Q water), 20 g 5% deactivated silica gel
(grade 923, 100–200 mesh; activated at 170 °C for 24 h) and finally
1 g anhydrous sodium sulfate. Small activated Cu pellets were
added to the top of the column to remove sulfur. The dichloro-
methane was replaced with n-hexane by elution, and the extract
was applied to the top of the column. The extract was eluted from
the column with 200 mL of 1:1 n-hexane–dichloromethane (pesti-
cide/PCB fraction). Extracts were then concentrated to 50 lL. Fi-
nally, 10 lL of tribromobiphenyl (5 ng lL1 in nonane) was added
as the injection standard before analysis.
2.3. Gas chromatographic analysis
OCPs and PCBs were analyzed separately with an Agilent 6890
Series GC System connected to an Agilent 5973 Network Mass
Selective Detector. Separation was accomplished with a DB-5 MS
fused silica capillary column (30 m  0.25 mm i.d., 0.25 lm film
thickness, J&W Scientific). Samples (1 lL) were auto injected in
splitless mode. The MS was operated in EI+ mode with selected
ion monitoring. For OCPs, the column flow was maintained at
1.0 mL min1 with the following temperature program: initial
oven temperature of 100 °C (1 min), ramping at a rate of
5.00 °C min1 to 200 °C (20.0 min), then to 250 °C (10.0 min) at
10.0 °C min1, and finally at 25.0 °C min1 to a final temperature
of 315 °C with a final holding time of 4.00 min. The injection port
temperature was maintained at 250 °C. PCBs were analyzed with
the following temperature program: initial oven temperature of
70 °C (2 min), ramping at a rate of 25.0 °C min1 to 150 °C
(0.0 min), then to 200 °C (0.0 min) at 3.00 °C min1, and finally at
8.00 °C min1 to a final temperature of 310 °C with a final holding
time of 6.00 min with the same flow rate and injector port temper-
ature as the OCP method. OCPs and PCBs were identified based on
the comparison of the retention time and mass spectrum of se-
lected ions with the calibration standards. Quantification was
accomplished through the application of a 8-point calibration
curve by running a series of standards containing the surrogate
standards (200 pg lL1), injection standards (0.020–1.00 ng lL1),
and native compounds (0.020–1.00 ng lL1). Relative response fac-
tors were derived for each compound and used to correct the peak
area for differences in ionization between analytes.
2469
2.4. Quality control procedures
Procedural blanks, field blanks, matrix spikes and duplicate
samples (10% of the analyzed samples) were carried throughout
the entire analytical procedure in a manner identical to the sam-
ples. Calibration standard were run at the beginning of each work-
ing day before each sample batch to establish the calibration
curves for the OCPs and PCBs. All samples were spiked with surro-
gate standards (see Section 2.2). Recoveries of the surrogate stan-
dards (n = 45) were 91.0 ± 6.78% and 94.4 ± 6.56% for OCPs and
PCBs respectively with a %RSD < 10. Sea sand (precombusted at
450 °C for 4 h) was used for the preparation of the matrix spike
samples (10.0 g), which was spiked at two levels (4 samples each):
0.200 ng g1 and 10 ng g1. Recoveries of the matrix spikes ranged
from 87.8%–107% and 91.2%–102% for OCPs and PCBs respectively
with a %RSD < 15. The method detection limits (MDLs) (Doong
et al., 2002) were determined as the concentration of analytes in
a sample giving a peak with a single-to-noise (S/N) of 3 and ranged
from 0.01–0.04 ng g1 for OCPs and PCBs. Concentrations of PCBs
and OCPs in the field and procedural blanks are in general <10%
of the amounts detected in any given sample, so results were not
blank corrected. To check for the validity of the method used for
the extraction and analysis of the sediment samples, a certified
reference material (NIST SRM 1941b) was analyzed in triplicates
during the analysis of samples and the recoveries ranged from
85.3%–101% for OCPs and 83.5%–108% for PCBs with RSD% < 20%
except for HCB (21.6%) and PCB 8 (22.4%). The values reported here
were not corrected for recoveries. All results were expressed on a
dry weight basis (dw), and those samples with concentrations less
than MDLs are reported as not detected (n.d.).
3. Results and discussion
3.1. Organochlorine pesticides
Concentrations of organochlorine pesticides in surface sedi-
ments from Lake Qarun are shown in Table 1. Endrin was the most
abundant compound in the sediment samples, followed by HCHs,
CHLs, aldrin, and endosulfans. Other OCPs such as DDTs, HCB, diel-
drin, endrin aldehyde, endrin ketone, and methoxychlor were
found at lower concentrations. The concentrations of different
OCPs had different spatial distribution. The significant difference
observed among the locations may be attributed to different input
source strengths, rates of degradation and sediment texture among
the locations (ATSDR, 1996), desorption and/or preferential sedi-
mentation (Iwata et al., 1994; Sericano et al., 2001; Martinez
et al., 2010). In general, higher concentrations of OCPs (with the
exception of HCHs) were found in sediments collected at stations
located near urban areas in the eastern and north-eastern region
of the lake. This result clearly indicates that urban areas of Faiyum
city are an important source of these compounds to the aquatic
environment of Lake Qarun. The organochlorine pesticides have
been banned from use and therefore, it is expected that the con-
centrations of these contaminants will decrease with time. Endrin,
HCHs, and endosulfans concentrations in Lake Qarun were higher
than those in most of the sediments collected from coastal areas
in Egypt (Barakat et al., 2002, 2012a,b) indicating local input
sources.
Among the cyclodiene pesticides and metabolites, aldrin had
the highest frequency of detection (95%), followed by endrin
(85%), dieldrin (76%), endrin aldehyde (32%) and endrin ketone
(23%). Endrin had the highest concentration in sediment samples
in all the studied areas with mean concentration of
20.4 ± 16.4 ng g1. Endrin appeared to be ubiquitously distributed
in the east and southeast coastal environment. Stations S17 and
S11 contained the highest concentrations of endrin (120.1 and
2470 A.O. Barakat et al. / Chemosphere 90 (2013) 2467–2476

Table 1
Concentrations (ng g1, dw) of PCBs and chlorinated pesticides in sediments at the study sites of Lake Qarun, Egypt (n.d., not detectable i.e., <detection limit).
P P
Station No. PCBsa ICESb DDTsc CHLsd HCB HCHse Aldrin Dieldrin Endrin Endrin Endrine Methoxy- Endo-
aldehyde ketone chlor sulfanf
S1 3.82 2.29 0.66 3.31 0.21 4.50 n.d. 0.50 19.1 n.d. n.d. n.d. 2.17
S2 28.9 5.69 1.81 3.38 0.14 0.70 3.26 0.52 11.3 n.d. n.d. n.d. 3.36
S3 51.2 14.7 0.19 0.82 n.d. 1.34 6.43 0.89 26.9 n.d. n.d. n.d. 0.97
S4 7.35 4.19 2.57 2.94 0.14 2.29 3.06 n.d. 14.3 n.d. 9.17 n.d. 4.20
S5 10.1 6.70 2.39 3.56 0.08 7.76 6.17 n.d. 18.8 n.d. n.d. 0.09 2.76
S6 10.3 4.54 0.53 2.61 0.11 34.8 2.10 1.23 13.3 10.2 2.05 0.02 1.62
S7 9.78 2.94 0.76 3.44 0.05 1.38 n.d. 3.20 9.60 n.d. n.d. 0.08 2.17
S8 2.92 1.45 n.d. 4.66 0.16 0.68 n.d. n.d. n.d. n.d. n.d. n.d. 1.85
S9 46.8 8.77 0.54 3.15 0.14 1.51 3.20 0.30 2.63 0.84 n.d. n.d. 1.20
S10 8.61 4.59 1.15 3.80 0.08 1.59 5.07 0.54 19.5 1.23 2.56 0.05 2.93
S11 107.5 45.9 1.23 5.31 0.12 1.17 0.81 3.41 112.4 n.d. 13.7 0.77 4.48
S12 10.0 6.61 3.38 2.72 0.06 3.39 11.5 0.27 24.6 n.d. n.d. n.d. 3.21
S13 7.57 2.54 2.55 2.74 41.2 1.36 0.32 0.23 37.6 n.d. n.d. 0.10 5.21
S14 17.9 2.96 1.11 3.12 n.d. 8.41 1.78 3.01 3.89 0.46 n.d. n.d. 1.84
S15 20.6 2.86 4.88 3.34 0.21 3.18 4.87 n.d. 75.0 n.d. 1.53 0.84 5.00
S16 137.2 65.1 5.88 3.64 0.07 2.22 5.76 2.53 18.7 4.27 4.10 0.19 4.31
S17 8.38 4.27 3.53 15.9 0.27 3.45 1.38 1.47 120.1 n.d. n.d. n.d. 18.7
S18 5.57 3.27 1.49 4.14 0.04 62.6 2.97 0.69 26.8 0.55 n.d. 0.19 2.03
S19 19.2 12.7 1.99 3.34 0.87 48.3 5.65 n.d. 17.7 n.d. n.d. 0.11 3.78
S20 3.27 1.34 0.14 0.25 n.d. 0.13 0.24 0.15 n.d. n.d. n.d. n.d. 0.13
S21 5.94 2.40 0.13 21.1 n.d. 0.81 7.98 2.22 n.d. n.d. n.d. n.d. 0.59
S22 1.48 0.90 0.51 0.31 0.13 0.19 0.44 0.33 6.13 n.d. n.d. n.d. 0.95
S23 2.47 n.d. 1.25 3.07 5.83 2.43 1.35 n.d. n.d. 1.01 n.d. n.d. 0.71
S24 10.6 3.31 1.57 3.17 0.04 2.59 0.67 0.14 7.98 n.d. n.d. n.d. 2.70
S25 6.69 4.44 1.63 2.25 0.05 4.37 0.81 1.05 5.62 n.d. n.d. 0.03 2.01
S26 7.89 4.42 0.89 0.77 0.04 1.55 0.46 1.03 3.76 0.19 n.d. 0.02 1.31
S27 4.12 2.16 1.19 0.26 0.05 1.00 1.10 n.d. 3.02 1.95 n.d. n.d. 0.89
S28 4.28 2.83 1.09 0.51 0.03 4.11 1.06 0.07 3.36 n.d. n.d. n.d. 1.04
S29 2.82 1.62 1.13 2.38 n.d. 100.6 2.25 1.00 n.d. n.d. n.d. n.d. n.d.
S30 15.3 7.25 0.31 2.83 0.10 0.76 12.2 5.36 21.0 n.d. n.d. n.d. 1.28
S31 11.9 4.32 2.14 2.04 0.47 3.55 2.03 0.42 3.02 1.33 1.61 0.04 1.81
S32 10.4 8.06 0.62 0.77 0.04 0.50 0.99 n.d. 3.44 0.25 n.d. n.d. 0.78
S33 10.8 7.48 2.02 2.41 0.04 10.8 3.68 1.18 13.1 n.d. n.d. n.d. 1.57
S34 11.5 4.97 0.99 2.63 0.09 0.92 3.26 1.76 52.0 n.d. n.d. n.d. 3.03
a
PCB represent the sum of 29 individual PCB congeners (IUPAC Nos. 8, 11, 18, 28, 44, 52, 66, 77, 81, 101, 105, 114, 118, 123, 126, 128, 138, 153 156, 157, 167, 169, 170, 180,
187, 189, 195, 206 and 209).
b P
7ICES is the sum of PCBs 28, 52, 101, 118, 153, 138 and 180.
c P
DDT is the sum of o,p0 + p,p0 forms of DDT and its breakdown products, o,p0 + p,p0 DDE and DDD.
d
CHLs is the sum of heptachlor and its epoxide, oxy-, cis-, and trans-chlordane, and trans-nonachlor.
e
HCHs is the sum of a-, b-, c-, and d-hexaachlorohexane.
f
Sum of endosulfan I, II and endosulfan sulphate.

112.4 ng g1, respectively). Station S17 is fairly close to El-Batts
drainage outflow while station S11 is in the vicinity of a minor
drain (Fig. 1). It is worth noting that there were significant differ-
ences in the content of endrin and its metabolites among the loca-
tion studied. Endrin undergoes photodegradation to endrin
aldehyde and endrin ketone (Nollet, 2000). Therefore, the abun-
dant levels of endrin in relation to its degradation products in
the sediment samples (Table 1) indicate recent input of endrin to
the aquatic environment of Lake Qarun.
Regarding the HCH compounds, the highest concentration were
found in samples collected from stations S29 (100.1 ng g1), S18
(62.1 ng g1), S19 (47.6 ng g1) and S6 (34.2 ng g1) while the
levels in the remaining stations were less than 10.7 ng g1.
Amongst the HCH compounds, c-HCH is the dominant isomer,
with a concentration range (0.09–100.1 ng g1), while a-HCH
(n.d. – 1.82 ng g1), b-HCH (n.d. – 0.44 ng g1), and d-HCH (n.d. –
1.40 ng g1) were present in minor amounts. The levels of HCH
isomers in sediment are shown in Fig. 2. On average c-HCH
accounted for about 95% of total HCH concentration in sediments.
The composition of organochlorines including some metabo-
lites can provide a tool for a better understanding of origin and his-
tory of input to the environment and possible degradation
pathways involved (Iwata et al., 1993). The typical technical HCH
generally contains a mixture of isomers, including 60–70% a, 5–
12% b, 10–12% c, 6–10% d, and smaller amounts of other isomers,
while lindane consists of 99% c-HCH (Iwata et al., 1993; Willett
et al., 1998). Hence, the ratios of a-HCH to c-HCH (a/c) would be
between 4 and 7 for the technical mixture and nearly zero for lin-
dane. In this study, a/c ratios ranged from 0 to 0.67 (with the
exception of sample S4, a/c = 2.03). Further, b-HCH was reported
to be the most stable isomer in HCHs because of its lower vapor
pressure, relative stability and resistance to microbial degradation
when compared to other isomers (Yang et al., 2005). Therefore, the
high abundance of this compound indicates past usage of HCHs
(Doong et al., 2002). Moreover, it should be noted that c-HCH
can be converted to a-HCH and subsequently to b-HCH (Wu
et al., 1997). In this study, the high abundance of c-HCH as com-
pared with a- and b-HCH, indicate that lindane has been most re-
cently used in these regions. Lindane has been one of the major
pesticides used to control cotton-boll worm in Egypt. Besides as
an agricultural insecticide, lindane has also been used as a pharma-
ceutical treatment for lice and scabies (Willett et al., 1998).
Total DDT tends to be elevated in areas near shore and is shown
to be ubiquitously distributed in the southeast urban region of the
lake (Table 1 and Fig. 1). The levels of DDT and its metabolites ran-
ged between n.d. – 4.28, n.d. – 0.75, n.d. – 1.12, n.d. – 1.64 and n.d.
– 0.40 ng g1 for p,p0 -DDE, o,p0 -DDD, p,p0 -DDD, o,p0 -DDT, and p,p0 -
DDT, respectively. The compositions DDT metabolites are shown in
Fig. 3. On average, metabolites accounted for 88% of total DDT,
implying substantial degradation of DDT. Among the metabolites,
p,p0 -DDE recorded the highest frequency of detection (97%),
followed by o,p0 -DDD (79%), p,p0 -DDD (72%), p,p0 -DDT (55%), and
 A.O. Barakat et al. / Chemosphere 90 (2013) 2467–2476 2471

α -HCH β -HCH γ -HCH δ -HCH

100%

80%

60%
Composition

40%

20%

0%
S1 S2 S3 S4 S5 S6 S7 S8 S9 S10 S11 S12 S13 S14 S15 S16 S17 S18 S19 S20 S21 S22 S23 S24 S25 S26 S27 S28 S29 S30 S31 S32 S33 S34

Station

Fig. 2. Percentage composition of HCHs in sediments from Lake Qarun.

o,p0 -DDT (28%). o,p0 -DDE was not detected in all the sediments
studied. Generally, the technical DDT contains 75% p,p0 -DDT, 15%
o,p0 -DDT, 5% p,p0 -DDE and <5% other (Yang et al., 2005). The
DDE/DDT ratio can be used to indicate whether DDT inputs have
occurred recently or in the past. Since p,p0 -DDE is a metabolite of
p,p0 -DDT (and is not present in technical DDT), lower and higher
ratios denote recent and past usage of technical DDT, respectively.
For example, it has been suggested that the ratios of (p,p0 -DDE +
P
p,p0 -DDD)/ p,p0 -DDT higher than 0.5 have been used to indicate
old input of DDT, while those less than 0.5 imply recent input
(Hong et al., 1999). Furthermore, Strandberg et al. (1998) also sug-
gested that ratios of p,p0 -DDT/p,p0 -DDE in sediments higher than
0.5 may indicate recent input of DDT, while the ratios less than
0.3 suggest past input. In this study, the ratio of (p,p0 -DDE + p,p0 -
P
DDD)/ p,p0 -DDT and p,p0 -DDT/p,p0 -DDE were in the range of
0.80–1.0 and 0.0–0.38, respectively; indicating that DDTs observed
in the present study area could be considered as past residue. On
the other hand, since p,p0 -DDT is degraded to p,p0 -DDE under aerobic

DDE DDD DDT

100%

80%

60%
Composition

40%

20%

0%
S1 S2 S3 S4 S5 S6 S7 S9 S10 S11 S12 S13 S14 S15 S16 S17 S18 S19 S20 S21 S22 S23 S24 S25 S26 S27 S28 S29 S30 S31 S32 S33 S34

Station

Fig. 3. Percentage composition of DDTs in sediments from Lake Qarun. DDE, DDD, and DDT are the sum of o,p0 + p,p0 forms.
2472 A.O. Barakat et al. / Chemosphere 90 (2013) 2467–2476
conditions and to p,p0 -DDD under anaerobic conditions (Aislabie
et al., 1997), the DDD:DDE balance may indicate the prevalent
conditions in the area. Consequently, the higher abundance of
DDE as compared to DDD in sediments from some locations of
the lake (Fig. 3) may reflect areas with lower organic inputs and
oxic conditions.
Chlordane related compounds were also detected in sediments
and ranged from 0.25 to 21.1 ng g1 with mean concentration of
3.55 ng g1 (Table 1). Among CHLs, heptachlor and oxy-chlordane
were the most abundant compounds in the sediment samples,
while the observed frequency and contents of trans-nonachlor
were the lowest. Oxy-chlordane varied from n.d. to 19.3 ng g1
with a detection frequency of 85% with highest concentration de-
tected at S21. Heptachlor (n.d. – 3.03 ng g1) was detected in all
sediment samples except for S11, whereas its photo-oxidation
product, heptachlor epoxide, ranged from n.d. to 1.89 ng g1 with
a detection frequency of 91%. The concentration ranges of trans-
chlordane and trans-nonchlor were n.d. – 0.35 ng g1 and n.d. –
0.23 ng g1 with detection frequency of 82% and 53%, respectively.
Heptachlor is itself a pesticide. It is rapidly degraded in the envi-
ronment to heptachlor-epoxide. Similarly, the components of tech-
nical chlordane, trans- chlordane, cis-chlordane and the
nonachlors are mainly degraded to the persistent metabolite oxy-
chlordane (Eljarrat et al., 2008). The metabolite products are often
more persistent and more toxic than their parent compounds. The
relatively high abundance of oxy-chlordane and heptachlor may,
therefore, indicate the presence of an aged mixture of CHLs and re-
cent inputs of heptachlor in the aquatic system of Lake Qarun.
Concentrations of endosulfan I, endosulfan II and endosulfan
sulfate were in the ranges of n.d. – 17.4 ng g1, n.d. – 12.4 ng g1
and n.d. – 0.68 ng g1, respectively. Endosulfan I, the most fre-
quently detected residue (97%), showed the highest mean concen-
tration (1.52 ± 1.37 ng g1) and was followed by endosufan II
(1.08 ± 0.56 ng/) with detection frequency of 82%, while endosul-
phan sulfate accounted for only 2.5% of the total endosulfans with
the lowest observed frequency and contents (15% and
0.07 ± 0.11 ng g1, respectively). Endosulfan sulphate is the major
degradation product of technical endosulfan which is a mixture
of the two isomers (endosulfan I and endosulfan II) in the ratio
of 70–80% to 30–20%, w/w, respectively (Leonard et al., 2001).
The trend in values of endosulphan isomers may therefore, sug-
gests recent input of technical endosulfan into the lake system.
Among other OCPs, the sediments at Lake Qarun contained
(with the exception of stations S13 and S23) relatively low HCB
residues, ranging from n.d. – 0.8 ng g1 with an average value of
0.12 ng g1. Significant concentrations of HCB, however, were
found in stations S13 and S23 (41.2 and 5.83 ng g1 dry wt., respec-
tively), indicating probable local sources at these locations. Resi-
dues of hexachlorobenzene (HCB) occur in the environment as a
result of its past manufacture and use as a pesticide and its forma-
tion as a by-product during the production of a variety of chlori-
nated compounds (Tanabe et al., 1997). Methoxychlor was rarely
detected in the samples and was only present at low concentra-
tions (Table 1).
3.2. Polychlorinated biphenyls
The total concentrations of PCBs (sum of 29 congeners) in sed-
iments ranged from 1.48 to 137.2 ng g1 with a mean value of
18.3 ± 16.6 (Table 1) indicating that PCBs are widespread contam-
inants in Lake Qarun. The PCBs concentrations are also expressed
P
as the sum of 7 individual congeners ( ICES, PCB IUPAC # 28,
52, 101, 118, 153, 138 and 180, Table 1) recommended by the
International Council for the Exploration of the Sea (ICES) in order
to harmonize data (Duinker et al., 1988). The distribution of RPCBs
indicates that areas of the Lake affected by urban and sewage dis-
charge are more prone to PCB contamination than other sampling
locations. Similar to the distribution of DDTs, concentrations were
higher at sampling sites close to urban areas. The highest level was
found at station S16 (Fig. 1), which is near to the outfall of El-Batts
drain, suggesting a possible localized pollutant discharge source.
The second highest PCBs contaminated location was station S11
(107 ng g1) close to a sewage outfall (Fig. 1). Elevated levels of
PCBs were also found at station S2, S3, S9 and S15 in close vicinity
to urban and sewage discharge (Fig. 1). Higher concentration of
PCBs in these locations suggests main input sources from areas rel-
atively close to municipal/industrial, and recreational regions.
Although the use of PCBs in Egypt as well as in other countries
has been banned currently, the past use of these substances in
transformers, electrical equipment, ship painting and other indus-
trial uses was common (Barakat et al., 2002). It is likely that the
PCBs came from the residues from former applications. There is
however no statistics on national imports (quantities or types) to
allow the estimation of potential volumes and sources of such uses.
The results from this study show that, owing to their persistence,
PCBs contamination is widespread in Lake Qarun.
Among the 29 PCB congeners analyzed, the maximum average
levels correspond to PCB 11 (di-Cl) and PCB 28 (tri-Cl), accounting
for 16% and 14% of the total PCB concentrations with detection fre-
quencies of 91% and 97%, respectively. PCBs 8 (di-Cl); PCB 18 (tri-
Cl); PCBs 52, 66 (tetra-Cl); PCBs 101, 126, 118 (penta-Cl) and PCBs
138, 153 (hexa-Cl) exhibited intermediate concentration levels.
The latter PCB congeners have low to medium toxicity levels
(Fernàndez et al., 1999). Finally, PCB 77, PCB 81, PCB 156, PCB
169 and PCB 105, the most toxic congeners analyzed, are present
at the lowest levels.
Typical chlorination level plots from the sediment samples are
illustrated in Fig. 4. Significant differences were observed in the
distribution profiles of PCB congeners according to the chlorine
substitution. With the exception of stations S2, S7, S9, and S14,
the PCB homolgues distribution shows that the relative composi-
tion of the PCB congeners was clearly dominated by the tri-, tet-
ra-, penta- and hexa-chlorinated biphenyls with these four
homologues representing 63–94% of the total amount of PCBs.
The type of pattern depicted in Fig. 4 is also similar to those ob-
served in different environmental compartments in Egypt (e.g.,
Barakat et al., 2002, 2012a,b). The PCB appears to be a mixture of
several aroclors (e.g., 1242, 1248, 1254). By contrast, the congener
patterns at stations S2, S7, S9, and S14 were largely dominated by
di-chloro congeners reflecting a contribution of a lower chlorinated
commercial formulation at these locations. The observed distribu-
tional variability of PCBs clearly reflects source differences, which
in most cases can be attributed to local point sources. However,
atmospheric transport of the lower chlorinated species and
the specific association of lower chlorinated congeners with the
sand-size fractions and of highly chlorinated congeners with the
finest fraction (Pierard et al., 1996) may also partly account for
the different pattern observed between the regions.
3.3. Comparison with previous work
The concentration ranges of PCBs, DDTs and HCHs in Lake
Qarun sediments are compared to those collected from different
rivers, lakes and estuaries worldwide in Table 2. The range of
PCB concentrations found in our study was one to two order of
magnitude higher than those generally reported in many river-
ine/estuaries systems worldwide, such in Yangtze Estuary, China
(Liu et al., 2003); Minjiang River Estuary, China (Zhang et al.,
2003); Danshui River Estuary, Taiwan (Hung et al., 2006); Bay of
Bengal, India (Rajendran et al., 2005); Hugli Estuary, northeast
India (Guzzella et al., 2005); estuarine and marine sediments,
Vietnam (Hong et al., 2008); Guba Pechenga and adjacent areas,
 A.O. Barakat et al. / Chemosphere 90 (2013) 2467–2476 2473

CL2 CL3 CL4 CL5 CL6 CL7 CL8-CL10

100%

80%
Composition

60%

40%

20%

0%
S1 S2 S3 S4 S5 S6 S7 S8 S9 S10 S11 S12 S13 S14 S15 S16 S17 S18 S19 S20 S21 S22 S23 S24 S25 S26 S27 S28 S29 S30 S31 S32 S33 S34

Station
Fig. 4. Percentage composition of PCBs in sediments from Lake Qarun.

Table 2
Comparison of organochlorine concentrations (ng g1 dw) in the sediments from other locations (n.d., not detectable (i.e., <detection limit); n.a., not available).

Location Year PCBs DDTs HCHs References

Asia
River and estuarine sediments from the Pearl River Delta 1996–1999 0.18–486 0.2–115.6 n.d. – 82.3 Fu et al. (2003)
Yangtze Estuary, China 2001–2002 0.19–18.95 (7 cong) 0.9–33.1 0.5–17.5 Liu et al. (2003, 2008)
Minjiang River Estuary, China 1999 15.14–57.93 (21 cong) 1.57–13.06 2.99–16.21 Zhang et al. (2003)
Baiyangdian Lake, North China 2007–2008 2.3–197.8 (12 cong) 1.3–51.3 4.7–679 Hu et al. (2010)
Danshui River Estuary and adjacent coastal areas, Taiwan 2001 and 2004 n.d. – 83.9 (209 cong) n.d. – 9.85 0.26–1.64 Hung et al. (2006, 2007)
Bay of Bengal, India 1998 0.02–6.57 0.04–4.79 0.17–1.56 Rajendran et al. (2005)
Hugli Estuary, West Bengal, northeast India 2003 0.18–2.33 (13 cong) 0.18–1.93 0.11–0.40 Guzzella et al. (2005)
Lower Mekong River Basin, Laos and Thailand 2005 0.18–310 (62 cong) 0.027–52 0.005–9.9 Sudaryanto et al. (2011)
Estuarine and marine sediments, Vietnam 2003–2004 0.04–18.71 (22 cong) 0.31–274 n.d. – 1.00 Hong et al. (2008)
Europe
Guba Pechenga and adjacent areas, Russia 1997 1.06–37.9 (11 cong) 0.27–36.7 0.05–0.68 Savinov et al. (2003)
Remote lakes and coastal areas, Norwegian Arctic 2005 0.18–13 (15 cong) 0.23–5.4 0.21–7.0 Jiao et al. (2009)
River Lambro, northern Italy 2001 10–3054 (Ar 1260) 1.5–167 0.5–27.6 Bettinetti et al. (2003)
Ebro River, Spain 1995–1996 5.3–17.7 (13 cong) 0.4–52 0.001–0.038 Fernández et al. (1999)
America
Lake Erie, Canada 1997 43 (av. of 24 cong) 8.0 (av.) n.a. Marvin et al. (2004)
Casco Bay, Maine, USA 2000–2001 0.3–148 (18 cong  2) 0.0–455.5 n.a. Wade et al. (2008)
Africa
Lake Victoria, Uganda 2003–2007 n.a. 4.24 ± 3.83 2.80 ± 2.00 Wasswa et al. (2011)
Lake Maryut, Egypt 2005 3.06–388 (96 cong) 0.07–105.6 n.d. – 2.20 Barakat et al. (2012a)
Lake Manzala, Egypt 2005 2.53–76.37 (96 cong) 0.20–5.17 n.d. – 3.42 Barakat et al. (2012b)
Lake Qarun, Egypt 2011 1.48–137.2 (29 cong) n.d. – 5.88 0.13–62.6 This study

Russia (Savinov et al., 2003); remote lakes and coastal areas,
Norwegian Arctic (Jiao et al., 2009); Ebro River, Spain (Fernández
et al., 1999); Lake Erie, Canada (Marvin et al., 2004); and Lake
Manzala, Egypt (Barakat et al., 2012b). Nevertheless, they were
comparable or slightly lower than several areas receiving substan-
tial anthropogenic inputs from urban and industrial activities, such
as Pearl River Estuary, China (Fu et al., 2003); Baiyangdian Lake,
North China (Hu et al., 2010); Lower Mekong River Basin, Laos
and Thailand (Sudaryanto et al., 2011); River Lambro, northern
Italy (Bettinetti et al., 2003); Casco Bay, Maine, USA (Wade et al.,
2008), and Lake Maryut, Egypt (Barakat et al., 2012a). Further,
the range of concentrations of RICES PCBs (n.d. – 65.1 ng g1)
was one order of magnitude higher than the estimated background
levels in Mediterranean sediments, i.e., 1–5 ng g1 (Gómez-Gutiérrez
et al., 2007a). These results indicate that contamination levels of
sedimentary PCBs in Lake Qarun can be categorized moderate to
high compared to other urbanized regions worldwide.
The DDT contents reported in this study are relatively low by
global standards and were in the same order of magnitude of the
estimated background levels in Mediterranean sediments i.e.,
0.08–5 ng g1 (Gómez-Gutiérrez et al., 2007a). When compared
with other studies, levels of DDTs in Lake Qarun exhibit similar val-
ues to those reported in Minjiang River Estuary, China (Zhang et al.,
2003); Danshui River Estuary, Taiwan (Hung et al., 2007); Bay of
2474 A.O. Barakat et al. / Chemosphere 90 (2013) 2467–2476

Table 3
Assessments of potential biological risks of selected OCPs in Lake Qarun using two sediment quality guidelines (NG: no guidline, n.d.: not detected).

Compound SQGsa (ng g1 d.w.) Study area Above ERLb (%) Above ERMb (%) Above TELb (%) Above PELb (%)
ERL ERM TEL PEL
P
PCBs 50 400 21.5 189 1.48–137 9 (3/34) – 15 (5/34) –
P
DDTs 3 350 NG NG n.d. – 5.88 12 (4/34) – NG NG
DDDc 2 20 1.22 7.81 n.d. – 1.87 – – 12 (4/34) –
DDEc 2 15 2.07 374 n.d. – 4.28 6 (2/34) – 6 (2/34) –
DDTc 1 7 1.19 4.77 n.d. – 1.64 3 (1/34) – 3 (1/34)
Endrin 0.02 45 2.67 62.4 n.d. – 120 86 (29/34) 12 (4/34) 83 (28/34) 9 (3/34)
Dieldrin 0.02 8 0.71 4.30 n.d. – 5.36 76 (26/34) – 41 (14/34) –
Lindane NG NG 0.32 0.99 0.09–100 NG NG 91 (31/34) 68 (23/34)
Heptachlor epoxide NG NG 0.60 2.74 n.d. – 1.89 NG NG 18 (6/34) –
Chlordanesd 0.5 6 2.26 4.79 n.d. – 19.4 68 (23/34) 6 (2/34) 9 (3/34) 6 (2/34)
a
SQGs Sediment Quality Guidelines, ERL effects low range, ERM effects median range (Long and Morgan, 1991; MacDonald et al., 2000); TEL threshold effect level, PEL
probable effect level (CCME, 2002).
b
Percentage of samples above the corresponding levels.
c
Sum of p,p0 - and o,p0 -isomers.
d
Sum of oxy-, cis-, and trans-chlordane.

Bengal, India (Rajendran et al., 2005); Hugli Estuary, northeast
India (Guzzella et al., 2005); Norwegian lakes and coastal areas
(Jiao et al., 2009); Lake Erie, Canada (Marvin et al., 2004); Lake
Victoria, Uganda (Wasswa et al., 2011), and Lake Manzala, Egypt
(Barakat et al., 2012b). Nevertheless, they are far lower than the
values measured in other heavily polluted areas, such as Pearl
River and Yangtze estuaries, China (Fu et al., 2003 and Liu et al.,
2008, respectively), Baiyangdian Lake, North China (Hu et al.,
2010); Lower Mekong River Basin, Laos and Thailand (Sudaryanto
et al., 2011); estuarine and marine sediments, Vietnam (Hong et al.,
2008); Guba Pechenga and adjacent areas, Russia (Savinov et al.,
2003); River Lambro, northern Italy (Bettinetti et al., 2003); Ebro
River, Spain (Fernàndez et al., 1999); Casco Bay, Maine, USA (Wade
et al., 2008), and Lake Maryut, Egypt (Barakat et al., 2012a). In
contrast, HCHs concentrations reported in this study were at the
higher values of the worldwide concentration range (Table 2).
3.4. Risk assessment of the persistent organochlorines in Lake Qarun
Gómez-Gutiérrez et al. (2007b) conducted a screening ecologi-
cal risk assessment (ERA) in the Mediterranean basin in order to
study the possible hazard induced by POPs contamination in mar-
ine sediments. According to their study, some areas of concern
were identified in the vicinity of certain industrial locations and
in the mouths of major rivers, spotting the need of further ecotox-
icological research in these zones in a detailed ERA. Moreover, the
study indicated that the toxicity induced by DDT in sediments
seemed to be the most important issue in the Mediterranean.
To evaluate the possible ecotoxicological risks of organochlo-
rine contaminants in the study area, concentration ranges of se-
lected analytes from the sampling location are compared to two
widely used sediment quality guidelines (SQG) for fresh water
ecosystems, i.e. the effects range-low value (ERL) and effects
range–median value (ERM) guidelines (Long and Morgan, 1991;
MacDonald et al., 2000) as well as the threshold effects level
(TEL) and probable effects level (PEL) guidelines from Canadian
Council of Ministers of the Environment (CCME, 2002). From the
data displayed in Table 3, it is apparent that the highest possibility
of occurrence of adverse ecological effects to benthic species is
associated with the exposure to c-HCH, which showed levels
higher than TEL and PEL values in 91% and 68.0% of stations,
respectively. Further, endrin and chlordanes were among the
investigated organochlorines that could pose occasional to fre-
quent adverse ecological effects to benthic species. As shown in
Table 3, concentrations of endrin exceeded the ERL and TEL values
in 86% and 83% of stations, respectively, among which 12% and 9%
of the stations also exceeded the ERM and PEL values, respectively.
Similarly for chlordanes, 23 sites (68% of stations) exceeded the
ERL value and 3 sites (9% of stations) exceeded the TEL value,
among which two of the sites also exceeded the ERM and PEL val-
ues. Lower possibility of occurrence of adverse ecological effects
was found to be associated with the exposure to dieldrin and hep-
tachlor epoxide, where 18–76% of stations exceeded the ERL and
TEL values for these contaminants, but none were found at concen-
trations at or above the ERM or PEL values. In the case of PCBs,
none of the stations exceeded the ERM and PEL values, but the sites
in proximity to the human activities exceeded the ERL guideline
value (i.e. stations S3, S11, and S16) and the TEL value (i.e. stations
S2, S3, S9, S11, and S16), which means that adverse effects on
aquatic biota may be expected to occur occasionally in these
locations. On the other hand, the concentrations of DDD, DDE,
and DDT were all below the ERM and PEL values, while one to four
sites (3–12% of stations) exceeded the ERL and TEL values for these
P
contaminants. For DDTs, 12% of the investigated samples collected
from sites in the near shore areas (i.e. S4, S5, S9, and S11) had
concentrations higher than the ERL value but lower than the ERM.
This suggested that adverse biological effects by DDT metabolites
would rarely or occasionally be observed in these locations.
4. Conclusions
The present study assessed the levels, distribution and toxico-
logical potential of OCs in sediments from various areas of Lake
Qarun, and add to the scarce knowledge of their environmental
distribution in lake sediments from Egypt. Due to a diversity of po-
tential inputs from sources such as industry, wastewater and sew-
age discharges, as well as agricultural runoff from the surrounding
drains, PCBs and OCPs contaminants are ubiquitously distributed
in sediments from Lake Qarun. The highest concentrations of OCs
were found at stations near agricultural runoff and municipal efflu-
ent discharges from urban areas of the city of Faiyum. The distribu-
tion of DDT and its metabolites suggest no recent inputs into the
lake environment. In contrast, recent input of lindane, endrin, hep-
tachlor and technical endosulfan to the aquatic environment of
Lake Qarun are apparent. Contamination levels of PCBs and HCHs
can be categorized as moderate to high in relation to similar areas
worldwide Based on the sediment quality guidelines, c-HCH, end-
rin and chlordanes would be more concerned for the ecotoxicolog-
ical risk in Lake Qarun. In addition; sediment concentrations for
PCBs, DDTs, dieldrin and heptachlor epoxide could potentially
cause occasional biological impairment. Therefore, source control
measures should be considered for protecting, or restoring,
 A.O. Barakat et al. / Chemosphere 90 (2013) 2467–2476 2475

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