Jan. 2008, Volume 2, No.1 (Serial No.2)
Journal of Environmental Science and Engineering, ISSN1934-8932, USA
Organochlorine pesticides in sediments from Honghu Lake, China
WANG Xiang-qin1,2, QI Shi-hua1,2, LI Jie1,2, LI Jun1,2
(1. Key Laboratory of Biogeology and Environmental Geology of Chinese Ministry of Education,
China University of Geosciences, Wuhan 430074, China;
2. School of Environmental Studies, China University of Geosciences, Wuhan 430074, China)
Abstract: The levels of 13 organochlorine pesticides (OCPs) in
sediments of Honghu Lake were investigated in order to evaluate
their potential pollution and risk. A total of 30 sediment samples
from 15 sampling locations were collected in the lake during July,
2005. The total concentrations in top-sediment samples and
sub-sediment samples ranged from 3.52 ng/g to 69.71 ng/g and
0.49 ng/g to 97.37 ng/g, respectively. The HCH isomers, DDT
congeners, aldrin, trans-chlordane, cis-chlordane, heptachlor and
endrin-ketone were significant in these samples. The
concentrations of OCPs in the lakeshore sediments were higher
than those sampled across the lake. Distribution of HCHs, DDTs
and other OCPs were different, indicating their various
contamination sources. Composition analysis in sediments
indicated recent usage or discharge of lindane, dicofol into the lake.
Key words: organochlorine pesticides; sediments; Honghu
Lake; China
1. Introduction
OCPs are among the most commonly detected
pesticides around the world. Although most were
banned decades ago, they can still be found in the
environment in several matrices such as surface water,
soil, river and marine sediments [1]. And due to their
volatility and persistence in the air, OCPs are subjected
to long-range atmospheric transport. Therefore, OCPs
released in the tropical and subtropical environments
could be dispersed rapidly through air and water, and
tend to be redistributed on a global scale [2-3].
Many developing countries are still using OCPs
for agricultural purposes due to their low cost and
 Acknowledgments:
The authors greatly appreciate the National
Basic Research Program of China for its financial support and
Doctor Julia for her kind help in modifying this paper.
WANG Xiang-qin (1982- ), female, graduate student; main
research field: environmental organic-chemistry. E-mail:
xiangqin109@163.com.
22
versatility in controlling various insects [4-5]. Surveys of
OCPs contamination have been reported in aquatic
sediments collected from Asian countries such as
Vietnam, Turkey, Korea and China indicating the
presence of significant levels of these pollutants in this
region [6,7].
In an aquatic environment, OCPs can enter marine
and freshwater ecosystems through effluents release,
atmospheric deposition, runoff and other means [8].
Due to their low water solubility, hydrophobic organic
contaminants in the water column generally tend to be
absorbed onto particulate materials and then find their
way to sediment as a sink. As a result, sediments in
aquatic environment have been recognized as the final
repository for these contaminants [9]. When disturbed,
the sediments can be resuspended, resulting in second
contamination. In terms of aquatic environmental
monitoring, the residues of OCPs reflect a recent
contamination [10]. Therefore, the investigation of
distribution of OCPs in sediments can indicate the
status of aquatic contamination [7,11,12].
Honghu Lake, the largest lake of Hubei Province,
is situated in China monsoon climate regions. It is
under strong influence of the Asian monsoon system. It
has an area of 355 km2, the distances from west to east
is 23.4 km and 20.8 km from north to south, the
maximum depth is 2.32 m and the minimum depth is
0.40 m, the floor of the lake is slightly tilted from west
to east. Many human activities have affected the lake
and its watershed: irrigation, aquiculture, fisheries,
shipping, inning, urbanization and the discharge of
sewage into the lake. In order to understand the
Organochlorine pesticides in sediments from Honghu Lake, China
pollution of OCPs in Honghu Lake, surveys were
carried out in the lake in 2005.
The objectives of this research are to (1) survey
the levels and distributions of OCPs in water and
sediments of Honghu Lake; (2) discuss the possible
sources of certain important OCPs.
Fig. 1
Table 1
Sample code
1
2
3
4
5
6
7
8
9
10
11
12
13
14
15
Longitude
11324.965
11324.666
11324.079
11322.915
11322.165
11321.479
11320.232
11319.019
11318.070
11315.588
11316.702
11318.058
11320.075
11321.961
11319.056
2.1 Sampling
Sampling locations
Coordinates of the sampling sites
Sampling sites
S01-1
S01-2
S01-3
S01-4
S01-5
S01-6
S01-7
S01-8
S01-9
S02-1
S02-2
S02-3
S02-4
S02-5
S02-6
2. Materials and methods
Latitude
2955.500
2954.477
2953.479
2951.538
2950.142
2948.618
2947.111
2945.804
2944.325
2953.848
2952.617
2951.727
2950.763
2949.990
2956.042
The locations of the sampling sites are shown in
Fig. 1 and Table 1. There are nine sampling sites along
the lakeshore and five sampling sites across the lake
from the entrance of the Yangtze River’s tributary to
the opposite lakeshore. Throughout the survey a Global
Positioning System (GPS) was used to locate the
sampling locations. At each site, one core was scooped
with a KC Kajak Sediment Core Sampler. Each core
was divided up into two layers, from the top layer (0-10
cm) the top-sediment sample was obtained and from
the sub layer (0-10 cm) the sub-sediment sample was
obtained, so there are 30 sediment samples in total. The
samples were sealed in polythene bags, air dried, then
passed through an 80 mesh sieve. All the equipment
23
Organochlorine pesticides in sediments from Honghu Lake, China
used for sample collection, transportation, and
preparations were free from organochlorines. Samples
were collected in July, 2005.
2.2 Extraction procedure
The soil samples were extracted using the
Soxhlet-extract method for 24 hours with
dichloromethane. A mixture of surrogate standards of
2, 4, 5, 6-tetrachlor-m-xylene (TCMX) and
decachlorobiphenyl (PCB209) were added to each of
the samples prior to extraction. Activated copper
granules were added to the collection flask to remove
any elemental sulfur. The extraction was concentrated
and solvent-exchanged to hexane and purified through
an 8 mm i.d. alumina/silica gel packed column from the
bottom to the top, with neutral alumina (3 cm, 3%
deactivated), neutral silica gel (6 cm, 3% deactivated)
and anhydrous sodium sulfate.
Before used, neutral alumina, neutral silica gel
were Soxhlet-extracted for 48 h with dichloromethane,
and then baked for 12 h in 240, 150℃, respectively.
Anhydrous sodium sulfate was baked for 4 h in 450℃
before using. The column was eluted with 50ml of
dichloromethane/hexane
(2:3)
to
yield
the
organochlorine pesticides fraction. The fraction was
concentrated to 0.5 ml by a rotary evaporator, and was
then concentrated to 0.2 ml under a gentle nitrogen
steam. A known quantity of pentachloronitrobenzene
(PCNB) was added as an internal standard prior to GC
analysis.
2.3 Instrument analysis
An HP6890 gas chromatograph equipped with a
Ni electron capture detector (GC-ECD) was used to
detect the levels of organochlorine pesticides in the
sediment samples. The capillary column ulitilized for
the analysis was a HP-5 (30 m×0.32 mm i.d. ×0.25 µm
film thickness). The oven heating regimen consisted of
raising the temperature from 100℃ to 200℃ at 4℃
min-1, then programmed to 230℃ at 2℃ min-1, then
programmed to 280℃ at 8℃ min-1 before holding for
15 minutes. Highly purified nitrogen was used as the
carrier gas at a rate of 2.5 ml min-1.2 µl as the extract
24
was injected into the GC-system in a splitless mode to
separate the OCPs.
A six point response factor calibration was
established to quantify the target analysis. The
OCP-residues were quantitatively determined by
comparing the area under each peak with the area under
the calibration peak. Two procedural blanks containing
all chemical samples were run to check for interference
and cross-contamination.
2.4 Quality assurance
For every set of ten samples, a procedure blank
and spiked sample consisting of all reagents was run to
check for interference and cross contamination. The
method detection limits (MLDs) of OCPs were
described as 3:1 signal versus noise value (S/N). MLDs
of OCPs ranged from 0.02 to 0.08 ng/g dry weight. The
spiked recoveries of OCPs using 50 ng of composite
standards were in the range of 78%-105%. The relative
standard deviation (RSD) ranged from 4% to 10%.
3. Results
OCPs detected in sediments included α-HCH,
β-HCH, γ-HCH, δ-HCH, heptachlor, aldrin,
trans-chlordane, cis-chlordane, p, p’-DDE, p, p’-DDD,
o, ’-DDT, pp-DDT and endrin-ketone. Total
concentrations of the13 organochlorine pesticides
ranged from 0.49 ng/g to 97.37 ng/g. Table 2 illustrated
the results of the sediment sample analysis and Fig. 2
illustrated the distribution of total OCPs residues in the
sediments of Honghu Lake. It revealed clearly that the
OCPs residues in the top-sediment samples were
comparable to the OCPs residues in the sub-sediment
samples. This meant there was no distinct degradation
trend from the top to the sub. Higher concentrations of
OCPs occurred in sediment samples which collected
along the lakeshore, which may be resulted from
farmland runoff, aquiculture, industrial sewage input
and other human activities near the lake. Lower
concentrations of OCPs occurred in sediment samples
which collected across the lake and may be due to a
Organochlorine pesticides in sediments from Honghu Lake, China
large flux dilution effect in the lake. It was observed
that DDTs concentration had positive correlation
relationship with OCPs, the correlation coefficient was
0.87. ∑other-OCPs (including heptachlor, aldrin,
trans-chlordane, cis-chlordane, endrin-ketone) had
significant correlation with OCPs, the correlation
coefficient is 0.99, too. But HCH content had no liner
relation with others.
Table 2 Range, mean and standard deviation (S. D.) of concentrations of
organochlorines (ng/g) detected in sediments of Honghu Lake
OCPs
α-HCH
β-HCH
γ-HCH
δ-HCH
∑HCHs
heptachlor
aldrin
γ-chlordane
α-chlordane
p,p’-DDE
p,p’-DDD
o,p’-DDT
p,p’-DDT
∑DDTs
Endrin-ketone
OCPs
Top-sediment samples
Range
Mean
0.04-5.11
0.56
0.03-0.47
0.24
0.03-2.29
0.61
0.05-15.00
1.85
0.54-16.36
3.25
0.06-4.85
1.07
0.09-9.09
1.25
n.d.-9.43
3.21
n.d.-15.21
3.43
0.09-2.04
0.8
0.01-1.37
0.38
n.d.-3.86
0.87
n.d.-2.78
0.44
0.89-7.91
2.49
0.49-25.76
3.74
3.52-69.71
18.45
S.D.
1.28
0.14
0.65
3.73
3.96
1.2
2.35
3.42
4.69
0.54
0.41
1.03
0.68
1.67
6.5
17.48
Sub-sediment samples
Range
Mean
n.d.-0.41
0.14
0.01-0.59
0.23
n.d.-2.22
0.61
0.10-1.62
0.54
0.13-4.79
1.52
0.02-5.68
1.02
n.d.-1.93
0.35
0.01-17.54
3.48
0.01-65.11
9.76
0.01-8.10
1.32
n.d.-6.73
1.05
0.01-2.25
0.60
n.d.-8.66
1.34
0.10-14.04
4.31
0.10-6.91
2.04
0.49-97.37
22.48
S.D.
0.12
0.20
0.76
0.45
1.48
1.56
0.51
4.85
17.82
2.05
1.95
0.63
2.35
4.51
2.61
27.62
α-chlordane, 0.01-8.8.10 ng/g for p, p’-DDE, n.d.-6.37
ng/g for p, p’-DDD, n.d.-3.86 ng/g for o, p’-DDT,
n.d.-8.66 ng/g for p, p’-DDT and 0.10-25.76 for
endrin-ketone.
4. Discussion
Fig. 2
Distributions of total OCPs in top-sediment samples
and sub-sediment samples
Concentrations of OCPs in sediment were
n.d.-5.11 ng/g for a-HCH, 0.01-0.59 ng/g for b-HCH,
n.d.-2.29 ng/g for r-HCH, 0.05-15.00 ng/g for d-HCH,
0.02-5.68 ng/g for heptachlor, n.d.-9.09ng/g for aldrin,
n.d.-17.54 ng/g for γ-chlordane, n.d.-65.11ng/g for
4.1 Residue levels of HCH and DDT in the
sediment samples
The composition differences for HCH isomers, or
DDT congeners in the environment may indicate
different contamination sources [11].
Concentrations of ∑HCH (ranged from 0.13-4.79
ng/g with a mean concentration of 1.52 ng/g) in the
sub-sediment samples were much lower than those for
∑DDT (0.10-14.04 ng/g with a mean concentration of
4.31 ng/g). This trend is consistent with the previous
observations on the contamination of OCPs in
sediments in China [8,13]. There was no quantitative
information to prove that the amount of technical HCH
25
Organochlorine pesticides in sediments from Honghu Lake, China
used was smaller than that of DDT. A most likely
explanation for the current relatively lower
concentrations of HCHs in sediments is due to the
differences in physicochemical and biological
properties, wherein HCHs have higher water solubility,
vapor pressure and biodegradability, and lower
lipophilicity and particle affinity compared to the
DDTs. DDTs tend to remain in the particulate phase
longer than HCHs [6].
But in the top-sediment samples, ∑HCH (ranged
from 0.54-16.36 ng/g with a mean concentration of
3.25 ng/g) were higher than ∑DDT (ranged from
0.89-7.91 ng/g with a mean concentration of 2.49
ng/g), which may be attributed to the relatively higher
vapor pressure of HCH [14] causing HCH volatize more
easily than DDT to the surface.
Table 3
Comparison of organochlorine residue levels (ng/g) in sediments collected from different aquatics
Location
Minjiang River
Qiantang River
Guangting Reservoir
Xiamen Western Bay
Jiulong River estuary
Pearl river estuary
Honghu Lake
HCHs
Range
2.99-16.21
8.22-152.1
n.d.-8.96
0.14-1.12
3.7-13
0.28-1.23
0.13-16.36
Mean
8.62
39.09
0.56
0.45
9.1
0.68
2.39
4.1.1 Composition of DDTs
Commercial grade DDT generally contains 75%
p, p’-DDT, 15% o, p’-DDT, 5% p, p’-DDE, <0.5% p,
p’-DDD, <0.5% o, p’-DDE and <0.5% unidentified
compounds [18], but in dicofol, the concentration of o,
p’-DDT is more than p, p’-DDT [19], A survey on the
formulated dicofol in the Chinese market found that the
ratio of o, p’-DDT to p, p’-DDT was as high as 7.0 [19].
Changes in the ratio of DDE and DDD to DDT
has been regarded as an indication of either no or
decreasing inputs to the environment [20]. The ratio of
(DDE+DDD)/∑DDT >0.5 can be thought to be
subjected to a long-term weathering [21]. More o,
p’-DDT than p, p’-DDT in the environment can
demonstrate the dicofol-type DDT usage [22].
26
The status of HCHs and DDTs contamination of
sediments in this study was compared with those in
other aquatics (Table 3). Total DDT levels ranged from
0.10-14.04 ng/g with a mean concentration of 3.20
ng/g. Such concentrations were lower than those in
Qiantang River, Guangting Reservoir, Xiamen
Western Bay and Jiulong River estuary. But they were
equal to those in Minjiang River and Pearl River
estuary. Total HCHs levels ranged from 0.13-16.36
ng/g with a mean concentration of 2.39 ng/g. Such
concentrations were higher than those in Guangting
Reservoir, Xiamen western Bay and Pearl River
estuary. They are equal to those in Minjiang River
estuary and Qiantang River.
DDTs
Range
1.57-13.06
1.14-100.2
n.d.-94.07
4.45-311
8.7-69
1.36-8.99
0.10-14.04
Mean
6.70
21.62
5.11
42.8
26
2.84
3.20
Reference
[12]
[8]
[15]
[16]
[17]
[16]
This study
In this study, the ratios of DDE plus DDD to DDT
(Table 4) in the top-sediment samples were between
0.12 and 82.56, in S01-8u, S01-9u, S02-1u, S02-2u,
S02-3u, S02-6u sampling sites the values were <0.5,
indicating that DDT-degradation little occurred in
these sampling locations. The predominance of the o,
p’-DDT-isomer and less p, p’-DDT isomer suggests
that there was extensive fresh input of DDT. But the
OCPs concentrations in most sites across the lake were
lower than those along the lakeshore (Fig. 2). So the
predominant may come from: (1) atmospheric
deposition. The atmosphere is known to be a source of
organic contaminants such as PCBs, HCHs, DDTs, and
chlordanes to large lakes [23,24]. The Asian monsoon
was supposed to have been playing an important role in
Organochlorine pesticides in sediments from Honghu Lake, China
the long-range atmospheric transport of POPs [2,4] and
Honghu Lake is situated in China monsoon climate
regions. It is under strong influence of the Asian
monsoon system. (2) dicofol application on fields near
the lake. In most top-sediment samples, the ratios of o,
p’-DDT to p, p’-DDT >1 indicated that dicofol was
being used in the Honghu Lake locality. Several recent
studies reported high DDT residues in sediments or
animal tissues, and revealed a new input of DDT,
especially in the South China [11]. For example, in the
Taihu Lake region, where the high concentration of o,
p’-DDT was attributed to the dicofol usage [25] and
dicofol application resulted in high DDTs residue in
cotton fields from northern Jiangsu province [26].
Further, According to Strandberg et al. [27], the ratio of
p, p’-DDT/p, p’-DDE provides a useful index in order
to know whether the DDTs at a given site were fresh or
aged. A value <0.33 generally indicates an aged input.
In this study, the values (Table 4) ranged from
0.02-9.35, with mean concentration of 2.67 and in most
sites it was more than 0.33, indicated there were fresh
inputs of DDT into the lake.
With regard to the sub-sediment samples, the
value of DDE plus DDD to DDT in the sub-sediment
samples was between 0.11 and 20.50 (with most values
being>0.62) showing that the degraded derivatives (p,
p’-DDD and p, p’-DDE) formed a significant
proportion of the total DDTs in the sub-sediment
samples. When talk to p, p’-DDT /p, p’-DDE, at most
sampling sites, the values >0.33 mean a fresh input of
that compound.
From above discussion, we know there is fresh
input of DDTs to the Honghu Lake. DDT-isomers have
a long persistence in the environment, gradually
degrading to DDE and DDD under both aerobic and
anaerobic conditions. The ratios of DDE to DDD can
indicate whether biodegradation of DDT occurred
under aerobic or anaerobic conditions. When aerobic
transformation is dominant DDE/DDD ratios are much
higher than one, while DDE/DDD ratios are close to
one under anaerobic conditions. DDT is
dehydrochlorinated
to
DDE
by
aerobic
microorganisms and therefore DDE/DDD ratio can
reach as high as 30 [28,29]. In irrigated soils and aquatic
environments, sediments can be submerged by
oxygen-depleted water so that reductive dechlorination
of DDT to DDD by anaerobic microorganisms would
be more favorable, decreasing the DDE/DDD ratios
[30]
. Previous use of technical DDD, however, can be a
confounding factor. DDD has insecticidal properties so
technical DDD was also used for agricultural purposes.
Therefore, DDD in the environment may have two
different sources, anaerobic transformation of DDT
and previous direct application of DDD. In recent
studies, the sediment samples have more DDD than
DDE usually [31]. The ratios of p, p’-DDE to p, p’-DDD
>1 (Table 4) in all of the samples, this phenomenon
consisted with the fact that the Honghu Lake has a
changeful water quantity along with the season, or may
be it was because that the DDTs in sediments could be
remobilized upward in the sediment core by
bioturbation [32], various kinds of marine benthic
organism, which accelerate the biodegradation process
of DDT to DDE, at the same time, the large quantity of
organic matter is also likely to play an important role
towards the degradation of DDT to DDE [33].
4.1.2 Compositions of HCHs
Technical HCH has been used as broad spectrum
pesticides for agricultural purpose, technical HCHs
consists principally of four isomers, α-HCH (55-80%),
β-HCH (5-14%), γ-HCH (12-15%) and δ-HCH
(2-10%) and other chloroorganic compounds [34], With
more than 99% γ-HCH in lindane [35]. Among these
isomers, α-HCH is more likely to be transported by air
for a long distance, β-HCH has the lowest solubility
and vapor pressure, which is the most stable and
relatively resistant to microbial degradation [36], the
properties of lower vapor pressure and less degradable
of β-HCH relative to other HCHs are accounted for the
elevated percentage of β-HCH. γ-HCH is unstable and
can be converted to a-HCH in the environment.
Therefore, the dominance of γ-HCH in the
27
Organochlorine pesticides in sediments from Honghu Lake, China
environment reflects the application of Lindane. After
long time aging, α-HCH and γ-HCH could be
transformed into β-HCH [37,38].
If technical HCH is the pollution source, the ratio
of α-HCH to γ-HCH should be 5.3-6.7. Therefore, the
α-HCH to γ-HCH ratio provided a method of
characterizing local lindane (almost pure γ-HCH)
release versus global transport of technical HCH
residues [39]. In this study, with regard to the
top-sediment samples and sub-sediment samples,
γ-HCH is the predominant HCH isomer in most
sampling sites along the lakeshore , the concentration
of γ-HCH ranged from n. d. to 9.43 ng/g with a mean
concentration of 3.21 in the top-sediment samples and
0.01 to 17.54 ng/g with a mean concentration of 3.48 in
the sub-sediment samples. γ-HCH is the predominant
HCH isomer in most sampling sites along the lakeshore
or near the entrance of brooks and tributaries of
Yangtze River, the γ-HCH residues contained in them
may have originated primarily from erosion of the land,
municipal sewage from local cities or from aquiculture
near the shore. The ratios of α-HCH to γ-HCH (Table
4) in the sub-sediment samples ranges from 0.09 to
2.63, which were much lower than 5.3, and in
top-sediment samples the value ranges from 0.07 to
9.63 ng/g with a mean concentration of 2.87, which
means there was lindane being input into the lake. The
results show that there are high concentrations of
δ-HCH in all top and sub sediments. Possible reasons
for the high δ-HCH concentrations are still unclear.
The phenomenon is similar to that of the sediment
samples from Guangting Reservoir in Beijing [40] and
the sediments of Xinghua Bay of Fujian province,
China [15].
4.2 Residue levels of other OCPs in sediments
The detection of aldrin and HCB in the sediments
showed that their contamination was wide spread
across Honghu Lake. It may have resulted from
agricultural runoff and wet deposition entering the
aquatic environment. It has been reported that HCB
and technical chlordane are still being extensively
28
produced in China to combat termites in buildings [41].
On the international market, technical chlordane is a
mixture of over 140 different components, the most
abundant of which are trans-chlordane (t-CHL, 13%),
cis-chlordane (c-CHL, 11%), heptachlor (5%) and
trans-nonachlor (5%), and the ratios of t-CHL/c-CHL
in technical chlordane are 1.2:1.0 [42]. Aldrin is still
extensively used in China [43]. Endosulfan is another
OCPs registered in China for the control of cotton
bollworm in cotton crops, and regarded as a “soft”
organochlorine due to its chemical properties,
degradation rate, and metabolism in plants and
animals[44]. Endrin is mostly represented in soils, due to
its low water solubility and vapor pressure [4], but there
is little endrin detected in the sediments. However, the
study showed that there is a large quantity of endrin
ketone in the sediments, possibly derived from endrin.
These
OCPs
(include
aldrin,
heptachlor,
trans-chlordane, cis-chlordane and endrin-ketone) have
never been used in large quantities in Hubei province,
but were detected in most sediment samples. The
results showed that these compounds probably
originated from other regional atmospheric flow
transport into Honghu Lake.
5. Conclusions
Thirteen OCPs were detected in the sediment
samples from Honghu Lake, due to several pathways
such as contaminants through the rivers, drainage from
the contaminated water off surrounding agricultural
fields, historic residues and atmospheric transport. The
concentrations of OCPs in the lakeshore sediments are
higher than those across the lake. Among these
pesticides, δ-HCH and o, p’-DDT were the two
dominant substances. Large quantities of γ-HCH
indicated there were lindane and dicofol were being
used in the Honghu Lake locality, respectively. OCPs
such as HCB, aldrin, heptachlor, trans-chlordane,
cis-chlordane and endrin-ketone have never been used
in large quantities in Hubei province, but were detected
Organochlorine pesticides in sediments from Honghu Lake, China
in most sediment samples. The results underscore the
need to improve environmental protection measures in
order to reduce the exposure of aquatic biota to these
persistent
and
bio-accumulative
compounds.
Furthermore, regular monitoring is required to evolve a
management strategy to ascertain environmental
hazards due to these OCPs.
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(Edited by Roy, Rita and Candice)