Environ Sci Pollut Res (2015) 22:2015420166

DOI 10.1007/s11356-015-5237-5

RESEARCH ARTICLE

Spatial distribution, source apportionment and ecological risk

assessment of residual organochlorine pesticides (OCPs)
in the Himalayas
Ningombam Linthoingambi Devi 1,2 & Ishwar Chandra Yadav 3 & Priyankar Raha 2 &
Qi Shihua 4 & Yang Dan 4

Received: 19 May 2015 / Accepted: 11 August 2015 / Published online: 25 August 2015
# Springer-Verlag Berlin Heidelberg 2015

Abstract The Indian Himalayan Region (IHR) is one of the

important mountain ecosystems among the global mountain
system which support wide variety of flora, fauna, human
communities and cultural diversities. Surface soil samples collected from IHR were analysed for 23 organochlorine pesticides (OCPs). The concentration of OCPs ranged from 0.28
to 2143.96 ng/g (mean 221.54 ng/g) and was mostly dominated by DDTs. The concentration of DDTs ranged from 0.28
to 2126.94 ng/g (mean 216.65 ng/g). Other OCPs such as
HCHs, endosulfan and heptachlor, Aldrin and dieldrin were
detected in lower concentration in IHR. Their concentrations
in soil samples ranged from ND to 2.79 ng/g for HCHs, ND to
2.83 ng/g for endosulfans, NDto 1.46 ng/g for heptachlor, ND
to 2.12 ng/g for Aldrin and ND to 1.81 ng/g for dieldrin.
Spatial distribution of OCPs suggested prevalence of DDTs

and HCHs at Guwahati and Itanagar, respectively. The close

relationship between total organic carbon (TOC) and part of
OCP compounds (especially - and -HCH) indicated the
important role of TOC in accumulation, binding and persistence of OCP in soil. Diagnostic ratio of DDT metabolites and
HCH isomers showed DDT contamination is due to recent
application of technical DDT and dicofol, and HCH contamination was due to mixture of technical HCH and lindane
source. This was further confirmed by principal component
analysis. Ecological risk analysis of OCP residues in soil samples concluded the moderate to severe contamination of soil.

Responsible editor: Hongwen Sun

Introduction

Electronic supplementary material The online version of this article

(doi:10.1007/s11356-015-5237-5) contains supplementary material,
which is available to authorized users.
* Ishwar Chandra Yadav
icyadav.bhu@gmail.com
1

Central University of South Bihar, BIT Campus,

Patna 800014, Bihar, India

Department of Soil Science and Agricultural Chemistry, Institute of

Agricultural Sciences, Banaras Hindu University, Varanasi 221005,
India

State Key Laboratory of Organic Geochemistry, Guangzhou Institute

of Geochemistry, Chinese Academy of Sciences,
Guangzhou 510640, China

State key Laboratory of Biogeology and Environmental Geology,

School of Environmental Studies, China University of Geosciences,
388, Lumo Road, Wuhan 430074, China

Keywords Organochlorine pesticides . Itanagar . Guwahati .

Tezpur . Dibrugarh

Organochlorine pesticides (OCPs) can be transported globally

due to semi volatile in nature, which has the capability to
move from warmer areas to cooler areas (Wania and Mackay
1993). OCPs such as dichlorodiphenyltrichloroethane, hexachlorocyclohexane, endosulfan, aldrins, dieldrin, heptachlor,
chlordane and other related compounds play an important role
in the contamination of environmental ecosystems (Deepa
et al. 2011; Bingham 2007; Gilliom et al. 2007; Oxynos
et al. 1989). These compounds have more capability to persist
for long time (UNEP 2002) and acute in living being (Colborn
1998; Dikshith et al. 1989). Due to the semi volatility and
persistence in nature, OCP used to detect at remote places
through long range atmospheric transport (LRAT) (Devi
et al. 2013). Although the productions and application of
DDTs and HCHs are banned in developed countries, still several developing countries including India involved in

Environ Sci Pollut Res (2015) 22:2015420166

productions and consumptions of DDTs and HCHs for domestic and agricultural purposes (Yadav et al. 2015)
Soil media act as reservoir of OCPs because of their long
time retention capabilities (Wang et al. 2012; Miglioranza
et al. 2003). Over the span of time, they can gradually be
changed from a major sink to an important emission source
of OCPs to food and drinking water. Substantial amounts (between 20 and 70 %) of OCPs and their degradation products
can remain in soil after their application. Today, majority of
pesticides used in agricultural fields are synthetic organic
compounds which may pass into the soil by missing their
intended target, released during spraying in plants or through
surface and subsurface runoff from agricultural field (Yadav
et al. 2015). The movement and accumulation of OCP in the
soil are governed by soil properties, chemistry of the OCP
compound, cropping system, irrigation pattern and climatic
conditions (Agnihotri et al. 1994). The physicochemical properties of the soil such as organic carbon, porosity, texture,
structure and moisture contain appear to control the fate and
persistence of the organochlorine compounds in soil (Backe
et al. 2004; Hippelein and Mclachlan 2000). Globally, organic
carbon present in soil plays a major role in the distribution and
persistence of OCPs in surface soil (Yang et al. 2012; Jiang
et al. 2009; Zhang et al. 2013).
Himalayas is the highest mountain range in the world and
has 9 out of 10 of the worlds highest peaks including Mount
Everest. The Indian Himalayan Region (IHR) is one of the
important mountain ecosystems among the global mountain
system (Singh 2006). Geologically, these are young mountains and are significant from the perspective of climate and
as a life support, providing water to a large part of the Indian
subcontinent (Bahadur 2004). Physiographically, it starts from
foothill of south mountain range to Tibetan plateau in north,
since IHR is very high altitude and is strongly influenced by
seasonal fluctuation (Wang et al. 2007, 2010; Chen et al.
2008; Chatterjee et al. 2010; Liu et al. 2010; Gong et al.
2014; Liu et al. 2014). Hence, there is much possibility that
the organic pollutants may get transported and accumulated in
IHR during monsoon especially Indian monsoon through
LRAT mechanism (Wania and Westgate 2008; Qiu 2013;
Gong et al 2014; Liu et al. 2014). Summer Indian monsoon
starts from July through September and enter India from
south-west part (Krishnamurthy and Kinter 2002). Hence,
the air mass filled with great amount of moisture brought by
both monsoon as well as indigenous moisture cause snow fall.
After September, as the sun start receding to south, the north
land mass in Indian subcontinent gets cool fast. This brings
cold wind from north part (Himalayas and Indo-Gangetic
Plain) to the greater part of South Deccan peninsula including
Indian Ocean (Nagarajan 2010). Long range transport and
atmospheric deposition of OCPs get seriously affected by
such Indian monsoon changes (Wania and Westgate 2008;
Chatterjee et al. 2010; Qiu 2013). Hence, understanding the

20155

fate and distribution of OCPs in IHR is matter of great

concern.
IHR has received much attention as it supports wide variety
of flora, fauna, human communities and cultural diversity
(Samant et al. 1998; Zobel and Singh 1997; Rao 1994). However, the role of IHR as recipient of POPs originating from the
plain is not much considered in the past. Recently, Mishra and
Sharma (2011) analysed human breast milk from Nagaon and
Dibrugarh and reported exceeding level of DDTs and HCHs.
They found that the local residents of the region are exposed to
high levels of OCP and stressed the need of detailed investigation and monitoring of OCPs in human and environmental
media. Furthermore, evidence suggests that toxic chemicals
are accumulating in the Himalayas and Tibetan Plateau (Qiu
2013; Sheng et al. 2013; Wang et al. 2006, 2007, 2008, 2010)
and stress the need of comprehensive study to assess the level
of organic pollutants in the region. To the best of our knowledge, studies on the assessment of OCPs residual level, their
distribution pattern and risk of OCPs from soil are very limited
in this region. Hence, present study aims to investigate the
occurrence, distribution pattern of OCPs and risk assessment
to ecological unities by residuals OCPs in surface soil from
IHR.

Materials and methods

Description of the study area
The study area (Guwahati, Tezpur, Dibrugarh and Itanagar) is
located in the eastern part of IHR. Guwahati, Tezpur and
Dibrugarh are the part of Assam (an Indian state) while Itangar
is the capital city of Arunachal Pradesh (another Indian state)
(Fig. 1). The Assam is located south of the eastern Himalayas
and comprises the Brahmaputra Valley and the Barak river
valleys along with the Karbi Anglong and the North Cachar
Hills. It is a temperate region and experiences heavy rainfall
and humidity. Guwahati, also the capital city of Assam, lies
between 26.11 N and 91.47 E. Tezpur is situated 175 km
north east of Guwahati and lies between 26.37 N and 92.50
E, while Dibrugarh is positioned 439 km east of Guwahati and
lies between 27.29 N and 94.58 E (Fig. 1). Itanagar lies
between 27.1 N and 93.62 E. The mean temperature ranges
between 13.5 and 27.5 C with lowest temperature in the
month of January. Annual rainfall in the area varies from
646 to 726 mm while relative humidity is around 88 %. Details description of sampling sites is presented in Table S1.
Sample collection
A total of 69 surface soil samples were taken and combined
into 23 composite samples. After all, 23 composite samples
were collected (depth ranging from 0 to 20 cm) from all four

20156

Environ Sci Pollut Res (2015) 22:2015420166

Fig. 1 Map of study area showing sampling locations

sites, namely, Guwahati (GS1, GS2, GS3, GS4 and GS5),

Tezpur (TS1, TS2, TS3, TS4 and TS5), Dibrugarh (DS1,
DS2, DS3, DS4, DS5 and DS6) and Itangar (IS1, IS2, IS3,
IS4, IS5, IS6 and IS7). Each sample was composite of three
sub samples. Stainless steel scoops were used to collect surface soil. The soil samples were then wrapped in aluminium
foil, packed into sealed polythene bags and kept in ice bag and
transported to laboratory. Hand gloves were used to avoid the
contamination during sampling. The soil samples were air

dried at room temperature. After proper drying, it was ground

to powder and sieved through 1-mm sieve and stored at 4 C
until analysis.
Physicochemical characterizations
Physicochemical parameter of soil samples was estimated immediately at laboratory of Soil Science and Agricultural
Chemistry, before storing in refrigerator. The pH and EC of

Environ Sci Pollut Res (2015) 22:2015420166

the soil samples were recorded using portable pH/EC metre

(HANNA, H198303). The colour of the soils was identified
by Munsell soil colour chart (Munsell 1973). The percentage
total organic carbon content in soil samples was analysed by
titrimetric method (Walkley and Black 1934; Jackson 1973).
Bulk density (BD) and particle density (PD) were determined
by pycnometer method (Black 1965). Water holding capacity
(WHC) of soil samples was determined by methods of Keen
box (Piper 1966).
Extraction and analysis
The required chemical reagents such as dichloromethane
(DCM), n-hexane and acetone were purchased from fisher
Scientific, USA and Tedia Co. USA. OCP standards 2, 4, 5,
6-tetrachloro-m-xylene (TCmX), decachlorobiphenyl (PCB
209) and 2, 2, 6, 6-tetrachlorobiphenyl (PCB54) were bought
from Ultra Scientific. All the glassware was dipped in
K2Cr2O7-H2SO4 solution for 24 h and cleaned before experimentation. About 10 g of well-dried and homogenized soil
samples were soxhlet extracted for 24 h with DCM as solvent.
Prior to extraction, a known amount of 20 ng of TCmX and
PCB209 was added as surrogate standards. Small chips of
activated copper were added to collection flask to remove
the elemental sulfur. After soxhlet extraction, the extract was
concentrated to about 23 mL by a rotary evaporator. The
extracted samples were cleaned by alumina/silica column.
The column was packed from the bottom to the top, with
neutral alumina (3 cm, 3 % deactivated), neutral silica gel
(3 cm, 3 % deactivated), 50 % acid silica (3 cm) and anhydrous sodium sulfate (1 cm). The column was eluted with
30 mL solvent of DCM/hexane (1:1). The eluted fraction
was concentrated and reduced to 0.2 mL on gentle nitrogen
stream. About 25 L of dodecane was added as a solvent
keeper. A known quantity of PCB-54 was added as an internal
standard prior to GC analysis. The eluted samples were
injected in to Agilent 6890A gas chromatograph equipped
with a Ni electron capture detector (GC-ECD). Details about
GC-ECD programme and injection time were described elsewhere (Devi et al. 2013).
Quality assurance and quality control (QA/QC)
After every ten samples, a set of calibration standards were run
to check for interference and cross contamination. Analytical
grade chemicals reagent was used in this experiment. Field,
procedural and solvent blank were examined by same procedure adopted for original sample analysis. The chromatogram
and peak of the blank solution and standard solution were not
overlapped and appeared clearly. The method detection limits
(MDLs) of OCPs were 3:1 signal versus noise value (S/N).
Surrogate recoveries in all samples for TCmX and PCB 209

20157

were 8015 %. OCP concentrations were expressed on dry

weight basis and were not corrected for recoveries.
Statistical analysis
Descriptive statistics, Pearson correlation and principal component analysis (PCA) were performed using IBM SPSS statistics (version 21). Samples with BDL concentration were set
as zero for calculation and analysis purposes.

Results and discussion

Physicochemical characterization
Physiochemical characterization of surface soil samples was
estimated and presented in Table S2. The majority of soil
samples collected from Guwahati, Dibrugarh and Tezpur
showed yellowish to light brownish in colour while soil samples from Itanagar exhibit brownish yellow, light brownish
grey, light grey, light yellow and yellowish brown colour.
Water holding capacity (WHC) of the soil samples ranged
from 27.5 to 48.8 % with mean 39.7 %. The BD and PD of
all the soil samples irrespective of study sites showed more or
less similar result and ranged 1.11.5 mg/m3 and 22.6 mg/
m3, respectively. The mean pH of soil samples (6.92) showed
slightly acidic in nature and ranged from 4.6 to 8.6. Percentage
TOC content in soil samples was detected low and ranged
from 0.4 to 2.5.
OCP level in surface soil
Descriptive statistics (min, max mean and SD) of residual
OCPs analysed in surface soil are presented in Table 1. Majority of the OCPs compounds were identified in surface soil
of IHR except endrin aldehyde, endrin ketone, cis-nonachlor
and methoxychlor. The OCP level in surface soil of IHR
ranged from 0.28 to 2143.96 ng/g. The OCPs concentration
measured in the present study was comparable with the OCPs
level observed in mountain forest soil in Czech Republic, but
far exceeding those in Mt. Qomolangma, China; Mount
Legnone, Italy; Pyrenees, Europe and Pico de Teide, Spain
(Table 2). Concentration of DDTs was higher than those of
HCHs, which is similar to many previous study reported in
mountain region of the world (Wang et al. 2007; Tremolada
et al. 2008; Xing et al. 2010; Holoubek et al. 2009; Gai et al.
2014). This is because the half-life of DDT (average 10
10.5 years) is more than the half life of HCH (average 20
50 days) (Harner et al. 1999). Therefore, DDTs are likely to be
more persistent and stay longer in soil as residues. Parent DDT
compound may degrade to DDE and DDD metabolites due to
photo-oxidation mechanism and are more persistent than parent compounds (Miejer et al. 2001). The DDTs accounted

20158
Table 1

Environ Sci Pollut Res (2015) 22:2015420166

Descriptive statistics of OCPs (ng/g)

Compounds

Minimum

-HCH

Isomer concentration of DDT and HCH

Maximum

Mean

Std. Dev.

ND

0.33

0.21

0.09

-HCH

ND

0.29

0.06

0.08

-HCH
-HCH

ND
ND

1.28
0.89

0.73
0.13

0.33
0.20

HCH
o,p-DDE

ND
ND

2.79
1.97

1.12
0.56

0.71
0.64

p,p-DDE

ND

78.8

15.9

28.4

o,p-DDD
o,p-DDT

ND
ND

10.5
484

1.60
36.9

2.61
115

p,p-DDD
p,p-DDT

ND
0.28

103
1448

13.6
148

30.4
355

DDT

0.28

2127

217

532

-Endo
-Endo

ND
ND

0.54
1.26

0.22
0.20

0.16
0.29

Endosulfansulfate
Endos

ND
ND

1.03
2.83

0.19
0.62

0.28
0.73

Heptachlor

ND

1.46

0.75

0.45

Aldrin
Heptachlor-epoxide
trans-Chlordane
cis-Chlordane

ND
ND
ND
ND

2.12
0.27
2.79
0.50

0.60
0.08
1.02
0.14

0.59
0.08
0.72
0.13

trans-Nonachlor
Dieldrin
Endrin
HCB
OCP

ND
ND
ND
ND
0.28

0.97
1.81
1.21
0.27
2144

0.10
0.11
0.31
0.03
221

0.23
0.40
0.30
0.06
537

ND not detected

for more than 97 % of total OCPs, while HCHs and

Endos accounted only 0.5 and 0.3 % of total OCP, respectively. The concentration of overall OCPs compounds was
highest in Guwahati and ranged from 1309.4 to 3695.2 ng/g
(mean 2502.2 ng/g), followed by 6 to 1705.7 ng/g in Tezpur
(mean 365.3 ng/g), 5 to 1834.2 ng/g in Itanagar (mean
312.8 ng/g) and 2 to 97.5 ng/g in Dibrugarh (mean
35.7 ng/g) (Table S3). The concentration of OCPs detected
at all sites of present study area is much higher than the
OCPs level observed in soil of other location than mountain
(Table 2), indicating towards accumulation of OCPs at high
mountain Himalayas. This is because larger precipitation
rates and reduced volatilization at high altitudes enhance
atmospheric deposition of OCPs at high-elevation sites
(Blais et al. 1998). The use of DDT (the major component
in OCPs) was banned in India in the year 1985 (Yadav et al.
2015). The high concentration of DDT together with moderate concentration of other OCPs in IHR suggests the
past use of OCPs compound and global distillation effect
in the region.

The concentration of OCPs analysed in surface soil from IHR

is shown in Fig. 2. Comparatively, the DDT (217 ng/g) and
HCH (1.12 ng/g) were most dominant OCP detected in soil
samples. The concentration of DDT observed at present
study area is several folds higher than reported in Mount
Legnone, Italy (2.2 ng/g) (Tremolada et al. 2008) and
Ruoergai highland, China (1.63 ng/g) (Gai et al. 2014). The
higher concentration of DDTs is also comparable with other
region of the world (Table 2). Elevated level of DDTs suggests
current use of DDT in IHR. High level of DDT in this studies
area probably because of DDT application in tea crop, because
this region is leading producer of tea (Devi et al. 2013). Another possible reason may because it is close to agricultural
field of West Bengal India (Chakraborty et al. 2010). The
DDT were likely to be transported a short distance from the
source through atmospheric deposition, because DDT have
short residence time and favour deposition in soil (Qiu and
Zhu 2010; Ricking and Schwarzbauer 2012). The most use of
DDT is because of an exception allowed for public health uses
in India. Several DDT metabolites such as p,p-DDT; o,pDDT; p,p-DDD; o,p-DDD; p,p-DDE and o,p-DDE were
also detected in soil samples. p,p-DDT (148 ng/g), o,pDDT (37 ng/g) and p,p-DDD (13.56 ng/g) were mostly dominant isomers found in present study. High concentration of p,
p'-DDT compared to o,p-DDT and p,p-DDD suggests fresh
input of DDT in current study area. The distribution of o,pDDT and p,p-DDD after p,p-DDT in the present area indicates active degradation of DDT in the soil and inputs of
already degraded DDT to the area (Hu et al. 2009).
The HCHs (1.12 ng/g) was the next most abundant OCP
after DDTs detected in soil samples of IHR. The observed
concentration of HCHs at present site is very much comparable with the HCHs level in Manipur (Devi et al. 2013) and
several high mountain region of the world (Table 2). However,
the HCHs level detected in IHR is much lower than Eastern
Tibetan Plateau, and Ruoergai highland in China (Xing et al.
2010; Gai et al. 2014). The elevated level of HCHs in this
study is may be because India is reported to be one of the
largest consumers of HCHs and most contaminated nations
in the world (Yadav et al. 2015). Paddy and cotton are the
two major crops grown India and requires about 29 and
27 % of the total pesticide consumption (Yadav et al. 2015).
Another possible reason was that HCHs used in other region
of India could be air transported and subsequently deposited
in IHR region (Wang et al. 2007; Xu et al. 2012). Among the
HCHs isomers, -HCH was most prevalent (0.72 ng/g) isomer detected in soil (Fig. 2). High concentration of -HCH is
indicative of presence of lindane contamination. The concentration levels of HCHs were observed in soils in the order HCH> -HCH>-HCH >-HCH. -HCH has the lowest water solubility and vapour pressure, which is the most stable and

Environ Sci Pollut Res (2015) 22:2015420166

Table 2 Comparison
table of DDT and
HCH in surface soil
(ng/g) around the world

20159

Country

DDT

HCH

Reference

Ruoergai highland

China

0.315.72

0.4310.6

Gai et al 2014

Manipur, Northeast India

India

0.495.68

0.012.85

Devi et al. 2013

Location
High mountain area

Eastern Tibetan Plateau

China

0.156.69

0.394.56

Xing et al 2010

Mountain forest soil

CzechRepublic

8.801908

0.261.66

Holoubek et al 2009

Mount Legnone

Italy

0.1811.0

0.011.88

Tremolada et al 2008

Mt. Qomolangma

China

0.396.06

ND

Wang et al 2007

Wolong

China

1.238.81

ND3.20

Zhang 2006

Pyrenees

Europe

1.703.40

0.080.19

Grimalt et al 2004

Pico de Teide

Spain

0.0140.0

ND1.00

Ribes et al 2002

IHR

India

0.282127

ND2.70

Present study

Hanoi

Vietnam

ND171

ND20.5

Toan et al. 2007

Hissar

India

0.0066.0

0.0051.0

Kumari et al. 2008

Guangzhou

China

7.60663

0.20104

Gao et al. 2008

KS Kaku
Chihuahua

Pakistan
Mexico

ND1538
1.00788

ND119

Syed and Malik 2011

Diaz-Barriga et al. 2012

Kurushetra

India

0.5037.0

0.608.50

Kumar et al. 2013

Korba

India

2.10315

0.9016.0

Kumar et al. 2014

Other location

ND not detected

relatively resistant to microbial degradation (Ramesh et al.

1991). Although the use of technical HCH was banned in
agriculture since 1997, but lindane is still allowed to use in
India in public health and in certain crop such as paddy rice
(Kumari et al. 2008; Kata et al. 2014; Yadav et al. 2015). The
presence of HCH and its isomers other than -HCH therefore
clearly indicates that these insecticides are still present in the
Indian environment.

Fig. 2 Concentration of DDTs and HCHs in surface soil

Spatial distribution of OCPs

The distribution of OCPs in surface soil from IHR is shown in
Fig. 3. Based on spatial distribution map, high concentration
of OCPs, especially DDTs, was detected at GS2 site in
Guwahati (mean 1837 ng/g) and the lowest concentration
was detected at DS2 site in Dibrugarh (1.41 ng/g) (Fig. 3).
High concentration of DDTs was found in soil samples mainly

20160

Environ Sci Pollut Res (2015) 22:2015420166

Fig. 3 Spatial distributions of OCPs (ng/g) in the Indian Himalayas Region

from Guwahati. This is because of famous tea crops and vegetables production in this region which relatively uses high
OCPs (Muraleedharan 2006; Gurusubramanian et al. 2008).
State of Assam including Guwahati is the worlds largest tea
growing region, producing more than 400 million
kilogrammes of tea annually (Asopa 2011). Highest concentration of HCHs (2.12 ng/g) was detected at GS4 site also in
Guwahati and lowest (0.08 ng/g) at DS5 site in Dibrugarh.
The concentration of HCH ranged from 0.52 to 2.12 ng/g
(mean 0.93 ng/g), 0.51 to 1.67 ng/g (mean1 17 ng/g), 0.08
1.44 ng/g (mean 0.91 ng/g) and 0.30 to 2.02 ng/g (mean
1.31 ng/g) in Guwahati, Tezpur, Dibrugarh and Itangar,
respectively.
Endosulfan is an organochlorine insecticide that was extensively used around the world to protect vegetables and fruits,
cotton and ornamental plants. It is banned in India because of
its high toxicities. The total concentration of endosulfan in the
soil samples ranged between 0.37 and 2.81 ng/g (mean

1.09 ng/g), 0.22 to 1.73 ng/g (mean 0.73 ng/g), 0.09 to

0.71 ng/g (mean 0.39 ng/g) and 0.09 to 1.74 ng/g (mean
0.64 ng/g) in Guwahati, Tezpur, Dibrugarh and Itanagar, respectively. The highest concentration of endosulfans was
found at Guwahati (Fig. 3). The concentration of -isomer
was higher than the -isomer in most of analysed soil samples
indicating the fast degradation of -endosulfan in soil.
Other OCPs such as aldrin, dieldrin and endrin are all cyclodiene chemicals and are lipophilic. The most common
source of general population expose to aldrin, dieldrin and
endrin is through contaminated food products grown in contaminated soil. Aldrin, dieldrin and endrin were detected low
in soil samples from all sites. The concentration of aldrin
ranged from 0.07 to 0.73 ng/g, 0.09 to 2.12 ng/g, 0.03 to
1.16 ng/g and 0.02 to 1.95 ng/g in Guwahati, Tezpur,
Dibrugarh and Itangar, respectively. This indicates the historical use of these compounds before they were banned in India.
This could also be due to transport of air mass from other

Environ Sci Pollut Res (2015) 22:2015420166

region by global distillation effect. Aldrin and endrin were

banned in 1996 and 1990, respectively, while dieldrin was
banned in 2003. Comparatively, higher concentrations of
Aldrin were detected in Tezpur.
Chlordane compounds are group of more than 140 different components which include trans-chlordane, cis-chlordane,
heptachlor and trans-nonachlor in major proportion. Heptachlor and chlordane are pesticides commonly used for termite
control. Heptachlor is also used in protecting plants seeds or
bulbs while nonachlor is a by-product of the manufacturing of
chlordane and heptachlor. In this study, concentration of heptachlor was most dominant among chlordane compounds in
all sites. The concentration of heptachlor ranged from 0.07 to
1.46 ng/g, 0.34 to 1.44 ng/g, 0.03 to 1.1 ng/g and ND to
1.18 ng/g in Guwahati, Tezpur, Dibrugarh and Itanagar, respectively. The concentration of trans-chlordane and cischlordane was found higher in soil samples from Itanagar
and is comparable with the concentration detected in soil sample from UK (0.051.6 ng/g and 0.071.0 ng/g) (Miejer et al.
2001) and USA (mean 0.49 and 0.43 ng/g) (Aigner et al.
1998).
Although HCB is not a registered pesticide in India, it
accounted about 30 % of total pesticides consumed in the
country (Yadav et al. 2015). The concentration of HCB was
detected low in all soil samples in the region. The highest
concentration of HCB was found in soil samples from Itanagar (0.27 ng/g).
Interrelationship of TOC and OCPs
TOC of the soil is an important factor that controls the fate and
distribution of OCP in soil (Yang et al. 2012). Organic carbon
in soil has affinity to bind OCPs because of their hydrophobic
nature (Jiang et al. 2009). Increase in organic content in soil
can provide more carbon source to microbial degradation of
OCPs. In present study, TOC content was positively and
weakly correlated with DDTs (r2=0.130) and HCHs
(r2=0.130) Fig. 4. Likewise, other OCP such as Endos and
Heptachlor were positively and weakly linked with TOC.
However, organic carbon was strongly and positively correlated with -HCH (r=0.765) and -HCH (r=0.612). The and -HCH isomers were weakly and positively correlated
with organic carbon (Table S4). This indicates the soil organic
carbon may increase the accumulation OCP in soil. Majority
of the DDT metabolite and other individual OCP compounds
were weakly and positively correlated with organic carbon.
This suggests other factors such as land use type, particle size
and soil chemistry may also contribute towards the retention
of individual OCPs in soil (Zhang et al. 2013; Jiang et al.
2009). Our findings are consistent with the previous studies
(Zhang et al. 2013; Mishra et al. 2012; Jiang et al. 2009).
Furthermore, p,p-DDE was strongly and positively correlated
with o,p-DDD (0.829), o,p-DDT (0.565), p,p-DDD (0.863)

20161

and p,p-DDT (0.811) (Table S4). -HCH was significantly

and positively correlated with HCB (0.683) and o,p-DDT
(0.731) suggesting similar sources of origin.
Source identification
The ratio of parent compound and their metabolite (also
known as diagnostic ratio (DR)) is used to identify the possible pollution source. p,p'-DDE and p,p'-DDD are the two
main metabolites of p,p'-DDT, and their ratio are used to investigate the extent of DDT degradation in the environment
(Eqani et al. 2011; Sarkar et al. 2008). DDTs are degradable
into DDD through reductive dechlorination under anaerobic
environment while into DDE under aerobic environmental
conditions. The DR of p,p'-DDT/(p,p'-DDD+p,p'-DDE) >1
indicate fresh application, while <1 suggest historical use. In
this study, the DR of p,p'-DDT/(p,p'-DDD+p,p'-DDE) was
>1 in all study sites and ranged from 2.42 to 6.45. This suggests recent use of DDT in the IHR. Technical DDT contain a
mixture of p,p'-DDT (about 85 %) and o,p'-DDT (about 15 %)
(Zheng et al. 2009). In order to know the contribution of
dicofol in total DDT, the DR of technical DDT and dicofol
(o,p'-DDT/p,p'-DDT) is used to estimate the source apportionment of DDT. The DR of o,p'-DDT/p,p'-DDT between 0.2
and 0.3 indicates the presence of technical DDT, while DR
between 1.9 and 9.3 or higher suggests contribution from
dicofol (Qiu et al. 2005). In the present study, the DR of o,
p'-DDT/p,p'-DDT ranged from 0.04 to 0.11 in all study sites
except Itanagar. The DR of o,p'-DDT/p,p'-DDT was 2 in Itanagar suggesting application of dicofol in the region. The DR
of p,p'-DDT/(p,p'-DDE+p,p'-DDD) and o,p'-DDT/p,p'-DDT
indicates that DDT contamination in the soil of IHR region
originated from recent application of technical DDT and
dicofol.
It is well known that the technical HCH contains -HCH
(about 6070 %), -HCH (about 212 %), -HCH (about 10
15 %) and -HCH (about 610 %). Technical HCH was
banned in India in 1996, but lindane is permitted to use in
public health sector and on some specific crops. The ratio of
-HCH/-HCH is used to indicate the source of pollution by
technical HCH or lindane. Generally, the ratio of -HCH/
-HCH greater than 4 is indicative of technical HCH contamination, while high -HCH percentage specifies lindane contamination (Kalantzi et al. 2001). In the present study, low
ratio of -HCH/-HCH was obtained in all sites and ranged
from 0.27 to 0.39. Also, higher percentage of -HCH (ranged
from 6674 %) and -HCH (2026%) showed that recent
application and transformation of lindane. Strong linkage between -HCH and -HCH observed in all soil samples reflect
the degradation of -HCH to -HCH (Walker et al. 1999).
Hence, it is concluded that the HCH in soil samples from
IHR originated from fresh application of lindane and limited
use of technical HCH.

20162

Environ Sci Pollut Res (2015) 22:2015420166

Fig. 4 Scatter plot of TOC with a

HCH, b DDT, c heptachlor and d
endosulfan

Technical chlordane was mainly used to control termite, to

control weeds in field and kill insects in soil. Normally, cischlordane to trans-chlordane ratio in technical chlordane
should be 0.79 (Rostad 1997; Dearth and Hites 1991). It is
fact that trans-chlordane degraded faster than cis-chlordane in
the environment. The cis-chlordane/trans-chlordane ratio >1
indicates the historical use of chlordane (Eitzer et al. 2001;
Bidleman et al. 2000). In our study, the ratios of cis-chlordane/trans-chlordane in soils were <1. This suggests the recent
application of chlordane in IHR region.
India is one of the largest producer and user of endosulfan
in the world (Wang et al. 2010). Technical endosulfan contains
about 70 % -endosulfan and about 30 % -endosulfan
(WHO 1984). The ratio of -endosulfan/-endosulfan <2.33
indicates the historical use of endosulfan whereas DR value
>2.33 specifies recent use. The -endosulfan decomposed
more easily than -endosulfan in soil. In our study, the DR
of -/-endosulfan ranged from 0.78 to 1.16 in Guwahati,
Tezpur and Itanagar indicating no fresh use of technical endosulfan. However, the DR value of -/-endosulfan at
Dibrugarh was higher (2.57) than 2.33 suggesting recent and
continual application of endosulfans in this study area.

Principal component analysis

PCA was also applied to estimate the source apportionment
and degradation behaviour of OCPs (Yang et al. 2008, 2012;
Jiang et al. 2009; Skrbic and Durisic-Mladenovic 2007). Seven major PC were extracted with Eigen value greater than 1
from all OCPs data which accounted for 86 % variance. The
factor loadings obtained after varimax orthogonal rotation
from OCPs data are given in Table S5. The degree of association between each variable showed the respective loading
factor for each component. PC1 explained 25.39 % of total
variance in OCPs data with strong positive loading on p,p
-DDE (0.964), o,p-DDD (0.840), p,p-DDD (0.858), p,pDDT (0.839), DDTs (0.892), endosulfansulfate (0.717) and
heptachlor (0.694). The high loading for DDTs and their metabolite suggests that they equally contributed to OCP and are
originated from similar sources. PC 2 which explained
16.95 % of total variance was associated mainly with
-HCH (0.599), -HCH (0.563) and -HCH (0.655), which
were also correlated with and HCHs (0.695). This indicates
the fact that the sources of HCH pollution in IHR are mixture
of both technical HCH and lindane. High loading on -, -and

Environ Sci Pollut Res (2015) 22:2015420166

-HCH can be explained by the isomerisation of -HCH

(Manz et al. 2001). PC 3 accounted for 15.48 % of variation
in OCPs data and was positively dominated by -endosulfan
and endos indicating the similar source of contamination.
PC4 represented 1.8 % of the total variance in OCPs data,
with high positive loading on -endosulfan (0.809), Aldrin
(0.594) and dieldrin (0.704). The loading plot of first three
components (PC 1, PC 2 and PC3) which explained 57 %
variation in OCPs data is shown in Fig. 5. It is evident from
Fig. 5 that heptachlor, heptachlor epoxide, cischlordane, endrin and trans-chlordane were separated from other OCPs
suggesting different source of origin. PC5, PC 6 and PC7
did not contain distinctive sources of variance in OCPs data
because of not having loading value greater than 0.50. Hence,
they are not considered and dropped from interpretation.

Ecological risk assessment

To assess the potential ecological risk of OCP residues, the
concentration of DDTs and HCHs in soil was compared with
the related soil quality guideline. Standard guidelines for
OCPs compounds in surface soil are not available in India.
Hence, our results are compared with the soil quality guidelines recommended by U.S. National Oceanography and Atmospheric Administration (NOAA), Canada government and
Chinese government. NOAA permits HCH level ranging from
50 ng/g in agricultural soil to 2000 ng/g in residential soil to
protect human health and environment (Buckman 1999). The
Canada government allows DDT concentration up to 700 ng/g
in residential and agricultural soil and 1200 ng/g in commercial and industrial soil. In our study, the level of HCH and
DDT was below the NOAA and Canada government recommended guidelines.

Fig. 5 Loading plot of first three major components (PC1, PC2 and PC3)
of PCA showing distribution of individuals OCPs

20163

The concentration of HCHs was observed in the present

study below the secondary standard value (500 ng/g dry wt.)
prescribed by Chinese government for safe agricultural farming (Wang et al. 2008). Likewise, DDTs concentration in all
soil samples except samples from Guwahati was below Chinese standard value. DDTs concentration in soil samples
from Guwahati (1249.2 ng/g) showed twice as high as Chinese standard value. This indicates that the soil at Guwahati is
contaminated with OCPs and is unsafe for agricultural farming. Similarly, primary standard values (50 ng/g dry wt. for
DDTs and HCHs) were set up by Chinese government to
protect environmental ecosystem and to maintain the quality
of background soil. In this study, six samples contained DDTs
higher level than the standard value. The level of HCHs in all
the soil samples was well within the limit of standard value.
The -HCH level in all samples was below the critical level of
40 ng/g dry wt. This suggests soil in the study area is less
contaminated with -HCH and is safe. The level of -HCH
and -HCH in all soil samples was below the critical concentrations of 100 and 10,000 ng/g, respectively, (Urzelai et al.
2000). Maximum concentration of DDTs allowed in soil is
10 ng/g in case of plant and invertebrate, 11 ng/g for small
birds and mammals and 190 ng/g for birds and animals (Qu
et al. 2015; Yu et al. 2013). In our study, the concentration
level of DDTs in eight soil samples were above the 11 ng/g dry
wt. limit, while only four samples exceed 190 ng/g concentration limit. Hence, it is concluded that the soil of the present
study area is partially contaminated with DDT and is modest
hazardous to plants, invertebrates, birds and mammal.

Conclusions
In the present study, high concentration of OCPs compounds
was detected in the soil samples. The concentration of OCPs
ranged from 0.28 to 2143.9 ng/g, which was higher than the
OCP residues reported in plain region of India; hence, indicating accumulation of OCPs in IHR. The concentration of DDTs
(mean 216.6 ng/g) was mostly dominated among all OCPs.
Elevated concentration of DDTs in IHR suggested the current
use of DDT because of an exemption allowed for DDT use in
public health. Spatial distributions of OCPs suggested the
prevalence of DDTs at Guwahati (mean 2502.2 ng/g), while
Itanagar detected maximum concentration of HCHs. TOC
content in soil samples was strongly and positively correlated
with -HCH (r=0.765) and -HCH (r=0.612) indicating the
role of organic carbon in accumulation of OCP in soil. Diagnostic ratio of DDT metabolite suggests the source of DDT
contamination in IHR due to recent use of technical DDT and
dicofol. The PCA analysis confirms the HCH pollution in the
IHR due to mixture of technical HCH and lindane. The ecological risk of the OCPs in soil samples was assessed based on
soil quality guidelines recommended by Chinese government,

20164

Canada government and NOAA. Based on NOAA and Canada government guidelines, the residual OCPs (DDT and
HCHs) in IHR may be classified as slightly contaminated
making them somewhat suitable for agricultural production.
However, the DDTs residue level in soil of Guwahati
exceeded the Chinese governments soil quality guideline indicating the severe contamination of soil.
Acknowledgement NLD is thankful to University Grant Commission
(UGC), New Delhi for financial assistance in the form of Dr. D.S. Kothari
Postdoctoral Fellowship.

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