Environ Monit Assess (2008) 136:239–244

DOI 10.1007/s10661-007-9679-1

Status of insecticide contamination of soil and water in Haryana, India

Beena Kumari & V. K. Madan & T. S. Kathpal

Received: 24 October 2006 / Accepted: 23 February 2007 / Published online: 4 April

2007
# Springer Science + Business Media B.V. 2007

Abstract Twelve samples each of soil and ground water were collected from paddy-
wheat, paddy- cotton, sugarcane fields and tube wells from same or near by fields
around Hisar, Haryana, India during
2002–2003 to monitor pesticide residues. Residues were estimated by GC-ECD and GC-
NPD systems equipped with capillary columns for organochlorine, synthetic
pyrethroid and organophosphate insecti- cides. In soil, HCH (0.002–0.051 μg g−1),
DDT (0.001–0.066 μg g−1), endosulfan (0.002–0.039 μg g−1) and chlordane
(0.0002–0.019 μg g−1) among organochlorines, cypermethrin (0.001–0.035 μg g−1)
and fenvalerate (0.001–0.022 μg g−1) among synthet- ic pyrethroids and
chlorpyriphos (0.002–0.172 μg g−1), malathion (0.002–0.008 μg g−1),
quinalphos (0.001–0.010 μg g−1) among organophosphates were detected. Dominant
contaminants were DDT, cyper- methrin and chlorpyriphos from the respective
groups. In water samples, HCH, DDT, endosulfan and cypermethrin residues were
observed frequently. Only chlorpyriphos among organophosphates was

B. Kumari (*) : T. S. Kathpal

Department of Entomology,
CCS Haryana Agricultural University, Hisar 125 004, India
e-mail: [email protected]

V. K. Madan
Medicinal and Aromatic Plants Section, CCS Haryana Agricultural University, Hisar
125 004, India
e-mail: [email protected]
detected in 10 samples. On consideration of tube well water for drinking purpose,
about 80% samples were found to contain residues above the regulatory limits.

Keywords Monitoring . Soil . Ground water . Gas liquid chromatograph (GLC) .

Multiresidues

Introduction

The agriculture sector is a very important part of the Indian economy. The
agriculture sector greatly con- tributes to the overall food needs of the country
and provides the domestic industry with agricultural raw materials. It promotes
industrial development through expanding the market for industrial goods such as
pesticides, chemical fertilizers, equipment and machines. Pesticides are generally
recognized as significantly benefiting our ability to meet the world’s need for
abundant, safe and affordable food and fiber. Pesticides reach the soil
environment by direct or indirect application from aerial and ground applica-
tions. The main processes potentially affecting the ultimate fate of pesticides in
soil are retention by soil materials (involving adsorption/desorption processes),
transformation processes (biological and chemical degradation), and transport
(through soil, atmosphere, surface water, or ground water) (Saltzman and Yaron
1986; van der Hoff and van Zoonen 1999). Several pesticides including
organochlorine, organophos- phate, carbamate and synthetic pyrethriod insecti-
240
Environ Monit Assess (2008) 136:239–244

cides, fungicides and herbicides are commonly used in vegetables and other crops
growing areas to increase the agricultural productivity. Pesticides enter surface
and ground water primarily as runoff from crops and are most prevalent in
agricultural areas. Although the use of such synthetic chemicals has led to
increased production of food and fiber but their use has also been associated with
several concerns, including risks to human health and alteration of local
environment (Calvert et al. 2001; Snodgrass
2001). The persistence of toxic pesticides in soil and water adversely affected
soil health (Kammenga et al.
2000), aquatic life and quality of drinking water
(Kumar et al. 1995). Contamination of soil and ground water has been reported
globally (Kumari et al. 1996; Bakra et al. 1990; Iwan 1988; Jani et al. 1991;
Ritter
1990). In US about 2% of wells in multi-state studies were found with pesticide
concentrations above the established maximum contaminant level (Barbash and Resek
1996). In this research, we conducted a moni- toring of multiresidues i.e.
organochlorines (OC), synthetic pyrethroids (SP) and organophosphates (OP) in soil
from different cropping pattern generally adopted in Haryana, Hisar, India and
ground water from tube wells to assess the contamination level and to plan the
future strategies for the safe use of pesticides.

Materials and methods

Sampling

Soil (1 kg) as well as water samples (1 l) were collected from the farmer’s field.
Soil samples were the top layers (15 cm) of soil obtained using stainless steel
auger at harvest from cotton-wheat, paddy-wheat cropping pattern and sugarcane
fields. Water samples were collected from the tube wells (20–60 m depth) of the
same or near by fields, periodically. The collected samples were kept in
refrigerator till analysis.

Extraction and clean-up

Pesticide residue extraction and clean-up was per- formed according to the
standard protocols.

Soil: Ground, sieved and dry representative (15 g) of soil sample was mixed
thoroughly with 0.3 g activated
charcoal, 0.3 g Florisil and 10 g of anhydrous sodium sulphate. The mixture was
packed compactly in a glass column (60 cm×22 mm) in between two layers of anhydrous
sodium sulphate. Pesticide residues were eluted with 100 ml of acetone: hexane
mixture (10:90v/v) at flow rate of 2–3 ml/min. Concentrated the eluate on flash
evaporator and made the final volume to 10 ml for GC analysis.

Water: Five hundred milliliter of water was taken in

1 l separatory funnel. Added 10–15 g sodium chloride and extracted with 15%
dichloromethane in hexane thrice (50, 30, 20 ml) by vigorous shaking. Organic
phase was collected, concentrated up to
10 ml and divided into two equal parts. One part was taken for estimation of OC
and SP insecticides whereas second part was processed for estimation of OP
insecticides. In both the cases, the solvent was evaporated to near dryness by
flash/manifold evapo- rator and the residues were redissolved in n-hexane for OC
and SP and in ethyl acetate for OP insecticides. Meticulous care was taken to
remove traces of dichloromethane from the extract used for estimation of OC and SP
insecticides.

Estimation

Samples were analysed for 26 pesticides including six organochlorines (HCH and its
four isomers, DDT and its five analogues, endosulfan and its three isomers,
heptachlor, aldrin and chlordane), four synthetic pyrethriods (cypermethrin,
fenvalerate, fluvalinate and deltamethrin) and seven organophosphates (chlor-
pyriphos, monocrotophos, dimethoate, methyl para- thion). The final extracts were
analyzed on Hewlett Packard 5890A gas liquid chromatograph (GLC) equipped with
capillary columns using electron capture detector (ECD) and nitrogen phosphorous
detector (NPD). Operating conditions were as per details: (1) for OC and SP
insecticides: detector: ECD (63Ni), column: SPB-5 of 5% diphenyl 95% dimethyl fused
silica capillary column (30 m×0.32 mm ID,
0.25 μm film thickness) with split system. Temper- atures: 150°C (5 min) at 8°C
min−1 to 190°C (2 min) at 15°C min−1 to 280°C (10 min), injection port 280°C,
detector 300°C; carrier gas: N2, flow rate 60 ml min−1, 2 ml through
column, split ratio 1:10. (2) For OP: Detector NPD, megabore column, HP-1
Environ Monit Assess (2008) 136:239–244
241

(10 m×0.53 mm ID, 2.65 μm) film thickness of methyl silicone. Temperatures:
Oven 100°C (1 min) at
10°C min−1 to 200°C (0 min) at 20°C min−1 to 260°C
(3 min), injection port, 250°C, detector 275°C, carrier gas N2, 1.8 ml min−1, H2,
1.5 ml min−1 and zero air
130 ml min−1.
The percent recoveries were in the range of 82–90,
75–92 and 90–98 at the fortification levels of 0.01–
0.10 μg g−1, 0.25 μg g−1 and 0.25–0.50 μg g−1 for
OC, SP and OP insecticides, respectively. Limits of detection (LOD) were 0.001 μg
ml−1/ μg g−1 for OC,
0.005 μg ml−1 for SP and 0.01 μg ml−1 for OP
compounds. Recoveries were considered satisfactory for all the insecticides in
soil and water with the proposed methods. Retention times and peak areas of
the studied pesticides were comparable with the relative standards. Accordingly,
the sample analysis data were corrected for these recoveries.

Results and discussion

Level of contamination of soil

Table 1 presents the levels of pesticide residues in 12 soil samples collected from
different cropping pattern. As evident from the data, all the samples were found to
be contaminated with OC compounds. Residues of HCH varied from 0.002 to 0.051 μg
g−1, DDT from
0.001 to 0.066 μg g−1 and of endosulfan from 0.002

Table 1 Monitoring of pesticide residues (μg g−1)* in soil under different

cropping system

Insecticide detected 1 2 3 4 5
6 7 8 9 10 11 12

α-HCH ND 0.003 0.003 ND ND

0.001 ND ND ND 0.003 0.001 ND
β-HCH ND 0.007 0.002 0.002 ND
ND 0.015 0.007 ND ND ND ND
γ-HCH 0.002 0.006 0.009 0.012 0.019
0.012 0.036 0.041 0.028 0.041 0.035 0.031
δ-HCH ND 0.003 ND ND ND
ND ND ND ND ND ND ND
Σ-HCH 0.002 0.019 0.014 0.016 0.021
0.013 0.051 0.048 0.030 0.044 0.036 0.031 o,p′-DDT
ND ND ND ND ND ND ND ND
0.001 0.005 ND ND p,p′-DDT 0.024 0.041
ND ND ND ND ND ND ND ND
ND ND o,p′-DDE 0.0006 0.007 0.005 ND
0.0006 ND ND ND ND ND ND ND p,p′-DDE
0.001 0.007 0.024 0.012 0.003 0.002 0.005 0.006
0.003 0.004 0.002 0.001 p,p′-DDD 0.002
0.011 ND ND ND ND ND ND ND
ND ND ND
Σ-DDT 0.027 0.066 0.029 0.012 0.004
0.002 0.005 0.006 0.004 0.009 0.002 0.001 α-Endosulphan
0.0006 0.004 0.016 0.008 0.002 0.003 0.004 0.003
0.009 0.010 0.009 0.013 β-Endosulphan 0.0002 0.006
ND 0.004 0.009 0.002 0.002 0.011 0.014
0.011 0.010
Endosulfan sulphate 0.001 0.029 ND ND 0.014 0.001
0.001 0.007 0.009 0.007 0.005 0.003
Σ-Endosulphan 0.002 0.039 0.016 0.012 0.025
0.006 0.007 0.010 0.029 0.031 0.024 0.026
Heptachlor ND ND ND ND ND
ND ND ND ND ND ND ND Aldrin
ND ND ND ND ND ND ND ND
ND ND ND ND Chlordane 0.0002 0.004
0.019 0.012 ND ND ND ND ND ND
ND ND Cypermethrin 0.004 0.001 0.004 ND
ND ND ND ND 0.026 0.035 0.027 0.021
Fluvalinate ND ND ND ND ND
ND ND ND ND ND ND ND Fenvalerate
0.002 0.013 0.002 ND 0.022 ND ND ND
0.003 0.007 0.005 0.001
Deltamethrin 0.018 ND ND ND 0.019
ND ND ND ND ND ND ND Chlorpyriphos
ND 0.019 0.172 0.137 0.026 ND ND ND
0.002 0.004 0.002 ND Monocrotophos 0.004 ND ND
ND ND ND ND ND ND ND ND
ND Dimethoate ND 0.002 ND ND ND
ND ND ND ND ND ND ND Me-Parathion
ND ND ND ND ND ND ND ND
ND ND ND ND Malathion 0.002 0.003
0.003 0.008 ND ND ND ND ND ND
ND ND Quinalphos 0.001 0.003 0.010 0.003
ND ND ND ND ND ND ND ND
Triazophos 0.010 0.010 ND ND ND
ND ND ND ND ND ND ND

*Average of two replicates

ND not detected
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Environ Monit Assess (2008) 136:239–244

to 0.039 μg g−1. γ-HCH among HCH isomers, p, p′ DDE among DDT analogues and β-
endosulfan among the endosulfan isomers were found to be the dominant contaminants.
Among other organochlorines, chlor- dane residues ranged from traces (0.0002 μg
g−1) to
0.019 μg g−1 in four samples where as heptachlor and
aldrin were not found in detectable levels in any of the samples. Although the use
of HCH and DDT are banned in agriculture since 1993 but lindane is still in use.
Presence of HCH and its isomers other than lindane (γ-HCH) and DDT analogues
clearly indi- cates that these insecticides are still lying in the
environment. Similar incidence of contamination of soil with OC insecticides in
world including India have been reported earlier also. Kumari et al. (1996)
reported the presence of HCH and DDT residues in soils collected from different
cropping regions of Haryana. Contamination of soil with DDT and HCH up to 0.675
and 0.032 μg g−1 , respectively has been reported from the states of Northern
India, i.e. Uttar Pradesh, Punjab and Delhi during 1965–1978 (Anonymous 1988). Thao
et al. (1993) demonstrated presence of HCH residues up to 0.005 μg g−1 and DDT
to the level of 0.0004 μg g−1 in Vietnam whereas HCH and DDT to the levels
of 0.020 and
0.083 μg g−1, respectively in Thailand. Hence our
results are in conformation with the earlier results. Organochlorines like HCH, DDT
and endosulfan have been reported in soils from Nicaragua (Carvalho et al.
1997) where their residue levels varied from 0.100 to
35 μg kg−1.
Among the four analysed synthetic pyrethroids, fluvalinate residues were not
detected in any of the samples. Cypermethrin ranged from 0.001–
0.035 μg g−1, fenvalerate from 0.001–0.022 μg g−1
and deltamethrin from 0.018–0.019 μg g−1 in 7, 8 and 2 samples, respectively.
Among the OP com- pounds, maximum contamination was observed with
chlorpyriphos, residues of which was detected in seven samples in the range of
0.019–0.172 μg g−1. Monocrotophos to the level of 0.004 μg g−1 and
dimethoate up to 0.002 μg g−1 was detected each in one sample. Residues of
malathion ranging from
0.002 to 0.008 μg g−1, quinalphos from 0.001 to
0.010 μg g−1 and triazophos from 0.010 to 0.010 μg g−1 were detected in 3, 4 and
2 samples, respectively. Similar to our results, residues of propanil, 2,4-D,
ethyl parathion, methyl parathion and chlorpyriphos
have been reported from soil of Guanacaste, Costa
Rica (Rodriguez 1997).
Presence of residues of SP and OP insecticides may be attributed to the change
in usage pattern of pesticides in agriculture sector of Haryana. In the past one
and half decade, the use of OC insecticides has been cut down drastically because
of their persistence in the environment. Mostly the shift has occurred in favour of
OP, SP and carbamate insecticides because of their wide spectrum of activity and
comparatively less persistence.

Level of contamination of water

All the 12 water samples collected from different tube wells were found
contaminated with HCH, DDT and endosulfan (Table 2). Among HCH, α-HCH, γ-HCH and
δ-HCH were found in detectable amounts. β-HCH was not detected in any
of the samples whereas one sample did not contain residues of any isomers of
HCH. ∑-HCH varied from 0.416 to
2.391 μg l−1 (ppb). Among DDT analogues, p, p′
DDT (0.032–0.703 ppb) was detected in all the samples and p, p′ DDE (0.009–0.162
ppb) in 11 samples. o, p DDT, o p, DDE and p, p′ DDD was found in 2, 1 and 6
samples, respectively. Residues of
∑-DDT ranged from 0.054 to 0.865 ppb. Residues of
∑- endosulfan varied from 0.023 to 0.371 ppb. α- endosulfan (0.003–0.142 ppb), β-
endosulfan (0.020–
0.288 ppb) and endosulfan sulfate (0.009–0.141 ppb) were present in most of the
samples. Aldrin, hepta- chlor and chlordane were not detected in any of the
samples. Maximum contamination was observed due to HCH, followed by DDT and
endosulfan. Observa- tions of the present studies clearly indicate that
organochlorine insecticides particularly HCH and DDT are still persisting in the
environment even after their restricted use/ban in agricultural and public sectors.
Among synthetic pyrethroids, only cyper- methrin in the range of 0.022–0.090 and
deltamethrin
0.017–0.061 ppb were detected in 6 and 4 samples, respectively. Residues of
chlorpyriphos only among OP compounds have been detected in 10 samples in the range
of 0.607–1.121 ppb. None of the samples contained other analysed organophosphates
like monocrotophos, dimethoate, methyl parathion, mala- thion, quinalphos and
triazophos in detectable amount. On adopting the European Union (EU)
Environ Monit Assess (2008) 136:239–244
243

Table 2 Monitoring of pesticide residues ((μg l−1)* or ppb) in ground water

Insecticide detected Tubewell

1 2 3 4 5 6
7 8 9 10 11 12

α-HCH 1.240 0.745 0.651 0.664 0.238

0.148 0.077 0.168 0.068 0.015 ND ND
β-HCH ND ND ND ND ND
ND ND ND ND ND ND ND
γ-HCH 0.878 0.885 0.541 1.674 0.537
0.689 0.592 0.563 0.432 0.425 ND 0.391
δ-HCH 0.241 0.342 0.074 0.053 0.031
0.153 0.073 0.165 0.045 0.061 ND 0.025
Σ-HCH 2.359 1.172 1.266 2.391 1.806
0.990 0.742 0.896 0.545 0.501 ND 0.416 o,p′-DDT
ND ND ND ND ND ND ND ND
ND ND 0.020 0.011 p,p′-DDT 0.703
0.190 0.204 0.188 0.254 0.215 0.222 0.193 0.169
0.173 0.040 0.032 o,p′-DDE ND ND ND
ND ND ND ND ND ND ND 0.010
ND p,p′-DDE 0.162 0.081 0.073 0.014 0.031
0.072 0.080 ND 0.009 0.013 0.020 0.011 p,p′-DDD
ND ND ND 0.115 0.044 ND 0.008 0.046
0.021 0.001 ND ND
Σ-DDT 0.865 0.271 0.277 0.317 0.329
0.287 0.310 0.239 0.199 0.187 0.090 0.054
α-Endosulphan 0.065 0.082 0.142 0.054 0.026
0.030 0.075 0.043 0.084 0.069 0.005 0.003
β-Endosulphan 0.141 0.051 0.038 0.045 0.218
0.288 0.142 0.037 0.020 0.121 0.030 0.020
Endosulfan sulphate ND ND ND 0.009 0.127
0.087 ND 0.141 ND 0.011 ND ND
Σ-Endosulphan 0.206 0.133 0.180 0.108 0.371
0.405 0.217 0.221 0.104 0.201 0.035 0.023
Heptachlor ND ND ND ND ND
ND ND ND ND ND ND ND Aldrin
ND ND ND ND ND ND ND ND
ND ND ND ND Chlordane ND ND
ND ND ND ND ND ND ND ND
ND ND Cypermethrin 0.030 ND ND 0.031
0.027 ND 0.022 ND ND 0.031 0.090 ND
Fluvalinate ND ND ND ND ND
ND ND ND ND ND ND ND Fenvalerate
ND ND ND ND ND ND ND ND
ND ND ND ND Deltamethrin 0.040 0.061
ND 0.031 ND ND ND 0.017 ND ND
ND ND Chlorpyriphos 1.000 0.791 0.812 1.121
0.912 0.607 0.871 0.810 1.001 0.791 ND ND
Monocrotophos ND ND ND ND ND ND
ND ND ND ND ND ND Dimethoate
ND ND ND ND ND ND ND ND
ND ND ND ND Me- Parathion ND ND
ND ND ND ND ND ND ND ND
ND ND Malathion ND ND ND ND
ND ND ND ND ND ND ND ND
Quinalphos ND ND ND ND ND
ND ND ND ND ND ND ND Triazophos
ND ND ND ND ND ND ND ND
ND ND ND ND

*Average of two replicates

ND not detected

permissible limit of individual pesticide in drinking water as 0.1 and 0.5 ppb for
total pesticides which has been currently been enforced in India (Anonymous
2003), residues in about 80% of the samples exceeded
the safe limits. Contrary to our results, higher residues have been reported by
Knedel et al. (1999) from watersheds of Motagua and Amatitlan comprising
sampling sites of rivers, lakes and drinking water, where total pesticide residue
levels reached up to 8 μg l1, the maximum level for organophosphates were
2.1 μg l−1 for cypermethrin 1.470 μg l−1 and for
organochlorines 0.56 μg l−1.Cypermethrin residues in
ground water samples from Guatemala used for human consumption exceeded safe levels
of 0.5 μg l−1 in most of the cases.

Conclusions

Soil as well as water (tube well) samples under paddy-wheat, cotton-wheat

and sugarcane fields have shown contamination with different groups of pesti- cides
which is a matter of concern. Regular monitor- ing of pesticide residues in soil
and water is required
244
Environ Monit Assess (2008) 136:239–244
in order to have a check on soil health and contamination level of water systems in
order to plan the future strategies for the use of pesticides.

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