Gas chromatographic analysis of pesticides in water

with off-line solid phase extraction

Tuija Pihlstrom
*
, Anna Hellstrom, Victoria Axelsson
National Food Administration, Box 622, S-751 26 Uppsala, Sweden
Received 1 April 1997; received in revised form 1 September 1997; accepted 7 September 1997
Abstract
A new solid phase extraction method has been developed to measure pesticide concentrations in water. The sample is extracted
using polymerdivinylstyrene extraction columns and eluted with ethyl acetate and injected in capillary gas chromatographic
columns connected to various detectors. Due to the very simple extraction procedure this method has a short analysis time.
The limit of quantication (LOQ) was from 0.05 to 0.1 mg/l depending on the pesticides to be analysed. The mean of the
recoveries for the method was 85%. The method was compared with liquidliquid extraction (LLE) in a study monitoring
pesticide residues in natural waters of Sweden. # 1997 Elsevier Science B.V.
Keywords: Gas chromatography; Pesticides; Solid phase extraction
1. Introduction
Several extraction methods for determination of
pesticides in water have been described [13]. The
conventional methods based on liquidliquid extrac-
tion (LLE) with dichloromethane have the disadvan-
tage that they are very time-consuming and also use
harmful chemicals.
The purpose of this study was to develop a rapid,
simple and sensitive gas chromatographic (GC)
method, in which only a few analytical steps are
needed for the determination of various pesticides
with a wide range of polarities (Table 1). The pesti-
cides studied are atrazine, desethylatrazine, desiso-
propylatrazine, dichlobenil, BAM, (2,6-dichlor-
benzamid, metabolite of dichlobenil), terbuthyl-
azine, bifenthrin, diazinon, metazachlor, dimethoate,
vinclozolin, fenitrothion, endosulfan-a, cyanazine,
chloridazon, l-cyhalothrin, cyuthrin-b and esfen-
valerate. This paper describes a gas chromatographic
method with solid phase extraction (SPE) using poly-
styrene-divinylbenzene sorbent, ENV extraction
columns. The obtained limit of quantitation (LOQ)
for the method was 0.05 mg/l for the pesticides studied
with the exception of the pyrethroids and BAM with a
quantication limit of 0.1 mg/l. Limit of detection
(LOD) ranged between 0.010.02 mg/l estimated from
standard solutions at a signal-to-noise ratio of 3 in GC
analysis. All these compounds have been used in
agricultural treatment in Sweden and are chosen on
the basis of their potential occurrence in Swedish
ground- and surface water.
Analytica Chimica Acta 356 (1997) 155163
*Corresponding author. Tel.: +46 (18) 175500; fax: +46 (18)
105848; e-mail: tuija@slv.se
0003-2670/97/$17.00 # 1997 Elsevier Science B.V. All rights reserved.
PI I S0 0 0 3 - 2 6 7 0 ( 9 7 ) 0 0 5 2 1 - 7
The method has also been applied to measure
pesticide residue levels in ground- and surface water
with incurred residues. During the recent years the
National Food Administration has investigated the
occurrence of pesticides residues in Swedish ground-
and surface water used for drinking supply [4]. The
annual samples from different Swedish water sources
were analysed by the solid phase extraction method
described here as well as with a liquidliquid partition
method. GC/MS was used for screening combined
with specic GC detectors for quantication.
2. Experimental
2.1. Extraction equipment
Isolute SPE columns, 1012 mm (internal volume
of 6 ml) containing 200 mg ENV

were purchased
from International Sorbent Technology (IST, Hen-
goed, UK). A VacMaster
TM
(IST, Hengoed, UK)
sample processing station was used to support the
columns during extraction.
2.2. Standards and solvents
Pesticide standards of analytical grade were sup-
plied by Dr Ehrenstorfer, Augsburg (Germany) and
Riedel de Haen, Seelze (Germany). Stock solutions of
standards were prepared in acetone. From those solu-
tions, mixtures of 36 pesticides were prepared based
on their chromatographic behaviour, except for
desethylatrazine and desisopropylatrazine which were
prepared as separate standard solutions due to the risk
of overlapping of the chromatographic peaks. Aliquots
of the mixture solutions were further diluted to
achieve spiking solutions (0.1 mg/ml) in acetone and
standards for GC calibration in ethyl acetate. The
stock solutions and all standard solutions were stored
at 48C. Acetone and ethyl acetate of pesticide quality
were used.
2.3. Extraction procedure for SPE
The extraction column was conditioned with 10 ml
ethyl acetate, 10 ml acetone and nally with 10 ml
water. An aliquot of 11 of water sample fortied with
pesticides was applied through the column with a ow
rate of ca 40 ml/min. The pressure, read on the Vac-
Master
TM
, was kept at 10 in. Hg (0.34 bar) and the
column material was not allowed to become dry.
Before eluting the pesticides, the column material
was dried by passing nitrogen for about 15 min.
Pesticides adsorbed were eluted with ethyl acetate
into a 5 ml calibrated volumetric tube until a nal
sample volume of 3.0 ml was achieved.
A nal volume of 3 ml is enough for a LOQ of
0.05 mg/l for most pesticides included, therefore no
evaporation is needed. If lower concentrations are to
be analysed, introduction of an additional concentra-
tion step can be used to improve detection limits.
Natural water samples have to be ltered through a
glass brelter before extraction to prevent clogging
of the adsorbent.
2.4. Chromatographic conditions
The gas chromatographic conditions used in this
study are according the National Food Administra-
tion's GC multi residue method [5,6] used for mon-
itoring pesticide residues in fruit and vegetables. The
sample extracts were analysed using a Varian Vista
6000 gas chromatograph equipped with a nitrogen
phosphorus detector (thermionic specic detector,
TSD) connected to a SE-30 fused silica capillary
column (CP-Sil 5 CB-MS) or to an OV-1701 (14%
cyanopropyl) capillary column (CP-Sil 19 CB) and a
Table 1
Water solubility of pesticides at 208C. Refer to C. Tomlin, The
Pesticide Manual, 10th edn. (1994)
Pesticide Watersol. mg/l Type
Esfenvalerate 0.002 (258C) Pyrethroid insecticide
Cyfluthrin-b 0.002 Pyrethroid insecticide
l-Cyhalothrin 0.005 Pyrethroid insecticide
Bifenthrin 0.1 Pyrethroid insecticide
Endosulfan-a 0.32 (228C) Organochlorine insecticide
Vinclozolin 3.4 Dicarboximide fungicide
Terbuthylazine 8.5 1,3,5-triazine herbicide
Dichlobenil 18 Benzonitrile herbicide
Fenitrothion 21 Organophosphorus insecticide
Atrazine 33 1,3,5-triazine herbicide
Diazinon 60 Organophosphorus insecticide
Cyanazine 171 (258C) 1,3,5-triazine herbicide
Chloridazon 340 Pyridazinone herbicide
Metazachlor 430 2-chloroacetanilide herbicide
Dimethoate 23 800 Organophosphorus insecticide
156 T. Pihlstrom et al. / Analytica Chimica Acta 356 (1997) 155163
Varian 3400 GC equipped with electron capture detec-
tors (ECD) and both a SE-30 fused silica and an OV-
1701 (14% cyanopropyl) capillary column tted to the
same injector.
A Hewlett Packard HP 5890 gas chromatograph
equipped with a quadrupole mass selective detector
(MSD) HP 5970 and a PAS-1701 (14% cyanopropyl)
capillary column was used to analyse BAM and to
screen for all pesticides in natural water. The dimen-
sions of all columns were 25 m0.32 mm I.D. OV-
1701 had a phase thickness of 0.20 mm, PAS-1701
0.25 mm and SE-30 had a phase thickness of 0.52 mm.
The following conditions were used for GC/TSD
and GC/ECD: splitless injection, 60 s; injection
volume 3 ml; carrier gas and make up gas, nitrogen;
injector temperature 2508C; detector temperature
2503008C. The temperature programme used: oven
temperature 908C held for 4 min, increased at 308C/
min to 1808C, increased at 48C/min to 2608C, and held
for 6 (TSD) resp. 12 min (ECD).
GC/MS conditions were as follows: splitless injec-
tion, 60 s; injection volume 2 ml; carrier gas helium;
injector temperature 2508C; transfer line temperature
2808C; ion source temperature 2002508C; ionisation
method electron impact; electron energy 70 eV, tem-
perature programme used: oven temperature 908C
held for 1 min, increased at 308C/min to 1808C held
for 0.5 min, increased at 108C/min to 2608C held for
10 min, increased 308C/min to 2808C, held 11.8 min.
Two ions for each pesticide were chosen for screen-
ing analysis in selected-ion monitoring (SIM)
(Table 2).
2.5. Recovery studies
Tap water was fortied with appropriate volumes of
standard solutions in acetone to get recoveries at the
levels 0.05 mg/l0.25 mg/l. In the rst assays, the
columns were chemically dried by adding acetone
in ethyl acetate as eluent (11). While changing
the eluent to pure ethyl acetate the column had to
be dried by passing nitrogen through it. In order to
determine the appropriate elution volume for the
pesticide studied, the elution prole was tested.
0.25 mg of pesticide to be analysed was added to 1 l
tap water. The sample was passed through the column
and eluted with acetone/ethyl acetate (11) collecting
ve fractions of 1 ml and one nal fraction of 2 ml.
All fractions were determined by means of GC/TSD
and GC/ECD. During the assay period, specicity
tests with blank water samples were performed regu-
larly. The method is shown to be selective towards
endogenous compounds with the exception of BAM,
which has been determined with mass selective
detection.
3. Results and discussion
For the analytical determination of pesticides two
different detectors were employed, TSD and ECD.
The nal results presented from GC/ECD analysis
(Table 3) are the mean values from separation on
SE-30 and OV-1701 columns. The concentrations
obtained with TSD are the mean values either on
SE-30 or on OV-1701 columns. Analyses of atrazine
and terbuthylazine are carried out either with SE-30 or
OV-1701. As shown in Table 4, different values were
obtained depending on the column. The breakdown
products of atrazine, desethylatrazine and desisopro-
pylatrazine were analysed only on SE-30 due to the
better chromatographic separation.
Table 2
Selected ions for SIM-detection and their limit of detection (LOD)
a
Pesticide Mass number LOD mg/l
Dichlobenil 171, 173 0.015
Diazinon 179, 304 0.09
Desethylatrazine 172, 187 0.045
Desisopropylatrazine 173, 158 0.06
Atrazine 200, 215 0.045
Terbuthylazine 214, 216 0.03
BAM 173, 189 0.045
Dimethoate 87, 93 0.06
Vinclozolin 212, 285 0.075
Fenitrothion 260, 277 0.09
Endosulfan-a 241, 339 0.11
Metazachlor 133, 209 0.11
Cyanazine 172, 198 0.15
Bifenthrin 166, 181 0.045
l-Cyhalothrin 181, 209 0.75
Chloridazon 221, 220 0.60
Cyfluthrin-b 226, 227 2.55
Esfenvalerate 225, 419 2.25
a
The limits of detection were estimated from injections of
standards (dissolved in ethyl acetate/cyclohexane, 11). A peak-
to-peak signal/noise ratio of at least 3 for the least intense ion for
each compound was required.
T. Pihlstrom et al. / Analytica Chimica Acta 356 (1997) 155163 157
Due to the water-immiscible elution solvent two
different drying procedures were studied. The use of
acetone as a drying agent was compared with blowing
nitrogen through the cartridge. In both assays water
samples were fortied with pesticides at levels of
0.050.25 mg. Mean values of the recovery tests for
all pesticides were 73% (acetone) and 85% (nitrogen).
The limit of quantication for the method was set in
most cases as the lowest concentration, where the
relative standard deviation (RSD) is estimated to be
less than 25%.
Very polar water miscible analytes, like dimethoate,
metazachlor and cyanazine, gave increased recoveries
when nitrogen was used as a drying agent. The mean
recoveries of these pesticides were 63% at 0.05 mg/l
level and 69% at 0.1 mg/l level using acetone/ethyl
acetate (11) as eluent, whereas with pure ethyl
acetate the mean recoveries were increased to 93
and 89%. Chloridazon was analysed by using only
acetone/ethyl acetate as eluent resulting in mean
recoveries of 78% of amounts added (0.050.25 mg)
(Table 3). According to previous studies [2,7,8], very
polar pesticides have caused problems when extracted
with silica-based sorbents like C
18
. In this study, the
extraction of very polar pesticides using the polystyr-
ene sorbent has been efcient.
Table 3
Recoveries obtained by using SPE and GC/ECD determination
EtOAc/Ac EtOAc
Pesticide Conc. mg/l n Recoveries % RSD % n Recoveries % RSD %
Dimethoate 0.05 4 81 12 3 113 19
0.1 14 64 25 3 80 1
Metazachlor 0.05 2 61 11 4 82 10
0.1 4 84 11 4 94 26
0.25 2 75 20
Cyanazine 0.05 2 46 11 4 83 7
0.1 4 58 31 4 93 14
0.25 2 60 28
Chloridazon 0.05 2 84 5
0.1 4 78 13
0.25 2 71 25
BAM 0.05 6 66 30
0.1 2 69 18
Diazinon 0.05 2 80 2 4 93 12
0.1 4 73 7 4 114 8
0.25 2 82 8
Dichlobenil 0.05 4 85 4 4 88 7
0.1 4 71 32 3 104 8
Endosulfan-a 0.05 4 76 16 7 80 25
0.1 13 104 23 5 117 18
Fenitrothion 0.05 4 83 8 7 103 14
0.1 13 63 27 5 88 17
Vinclozolin 0.05 4 78 21 6 102 12
0.1 9 96 24 1 107
Cyfluthrin-b 0.05 4 53 6 4 49 8
0.1 11 54 22 6 67 24
l-Cyhalothrin 0.05 4 51 13 3 57 4
0.1 10 56 26 5 62 22
Esfenvalerate 0.05 4 44 14 4 53 12
0.1 10 44 23 5 70 10
Bifenthrin 0.05 4 49 14 3 48 2
0.1 11 52 19 4 75 12
Mean values 69 17 83 14
158 T. Pihlstrom et al. / Analytica Chimica Acta 356 (1997) 155163
The pyrethroids, cyuthrin-b, l-cyhalothrin, esfen-
valerate and bifenthrin, showed recoveries of 4453%
when 0.05 mg was added and acetone/ethyl acetate
was employed as eluent. The recoveries were not
signicantly higher at this level eluting with pure
ethyl acetate. On the other hand, at the higher level
increased recoveries were obtained with ethyl acetate.
With respect to the hydrophobic character of pyre-
throids, the poor recoveries of these analytes might be
due to difculties in elution rather than in retention.
Semipolar pesticides gave acceptable results in both
studies except for BAM. The measured concentrations
were less than 70% quantied with GC/MS (SIM). In
the preliminary recovery tests (not reported here),
BAM was measured with ECD. Due to the occurrence
of overlaying components produced with ECD, spe-
cially in natural waters, the evaluation of BAM caused
problems. Therefore, it was crucial to make use of the
SIM technique, which provided a conrmation and
quantication of BAM.
Table 4
Recoveries of terbuthylazine, atrazine and its breakdown products obtained with GC/TSD determination
Pesticide EtOAc/Ac EtOAc
Column Conc. mg/l n Recoveries % RSD % n Recoveries % RSD %
Atrazine SE-30 0.05 4 122 43
0.1 6 60 17
OV1701 0.05 6 59 13
0.1 7 128 9 5 86 33
Desethylatrazine SE-30 0.05 2 98 4 3 113 4
0.1 6 80 55
Desisopropylatrazine SE-30 0.05 2 99 6 3 100 29
0.1 6 56 65
Terbuthylazine OV1701 0.05 2 53 16 4 99 9
0.1 2 106 1 3 95 6
SE-30 0.05 2 90 7
0.1 4 61 36
Mean values: 87 24 92 16
Table 5
Elution profiles of 0.25 mg pesticides added on the ENV

. Eluent: acetone/ethyl acetate

Pesticide Fractions (ml), recoveries (%) Total recovery
(%)
Loss of recovery
collecting 3 ml (%)
01 12 23 34 45 57
Cyanazine 103 4 0 0 0 0 107 0
Chloridazon 64 24 13 7 3 2 113 10.6
Metazachlor 83 19 0 0 0 0 102 0
Dichlobenil 67 1 0 0 0 0 68 0
BAM 49 10 5 4 2 1 71 9.8
Dimethoate 92 12 2 0 0 0 106 0
Vinclozolin 74 15 9 7 3 2 110 10.9
Fenitrothion 58 7 3 5 1 1 75 5.3
Endosulfan-a 65 19 8 5 3 1 101 8.9
Diazinon 94 4 0 0 0 0 98 0
Atrazine 74 19 8 3 2 1 107 5.6
Bifenthrin 62 26 9 4 1 0 102 4.9
l-Cyhalothrin 85 28 9 3 1 0 126 3.2
Cyfluthrin-b 82 28 11 4 0 0 125 3.2
Esfenvalerate 77 29 10 3 0 0 119 2.8
T. Pihlstrom et al. / Analytica Chimica Acta 356 (1997) 155163 159
The mean recoveries of the other semipolar pesti-
cides were improved from 80% to 100% by eluting
with ethyl acetate. In conclusion, ethyl acetate elution
is more efcient with ethyl-acetate than with acetone/
ethyl acetate and is therefore recommended.
Elution proles were studied in order to achieve the
sufcient elution volume needed for the method (see
Table 5). The average loss of recoveries, collecting
totally 3 ml, was 4%. Since the quantication limit of
0.1 mg/l required by the E.C. Council Directive for
water could be achieved without an additional con-
centration step, the nal sample volume was deter-
mined to be 3 ml.
4. Comparison of LLE and SPE analysing
incurred water samples
4.1. Sampling
Water samples were collected in 1 l glass bottles
ushed with acetone and equipped with PTFE teon-
coated screw caps. To preserve the samples, 30 ml
dichloromethane was added to the samples intended
for LLE. All samples were stored at 48C and analysed
within 24 h of reception.
4.2. General procedure
Slightly more than 100 samples from different
water supplies were analysed using two different
extraction procedures. The liquidliquid solvent
extraction employed in this study was based on the
distribution of solutes in dichloromethane whereas the
solid phase extraction procedure used has been
described above. The contents of pesticide residues
were investigated with both methods.
4.3. LLE extraction procedure
The liquidliquid method used is, with slight mod-
ications, equal to the method reported by A

kerblom
et al. [3]. The water samples were extracted three
times with dichloromethane containing sodium chlor-
ide for salting out. Water was removed using sodium
sulfate. Dichloromethane was replaced by ethyl acet-
ate and concentrated in a rotary vacuumevaporator. To
avoid losses of pesticides during the evaporation,
some portions of ethyl acetate were added prior to
the removal of dichlormethane. The nal volume was
adjusted to 3.0 ml with ethyl acetate. The clean-up
step with gel permeation chromatography was
excluded in this study, because interfering peaks in
chromatograms appeared to be absent. However, we
will point out that the quantication of BAM in both
extraction methods has been done with SIM due to an
overlapping endogenous peak.
4.4. Results
Altogether there were 106 analysed ground- and
surface water samples, originating from different geo-
graphical areas in Sweden. In cases where the ground-
or surface water contained pesticide residues, a drink-
ing water sample from the same catchment was exam-
ined.
The pesticides determined with both these methods
were atrazine and its two breakdown products,
desethylatrazine and desisopropylatrazine, BAM
(metabolite of dichlobenil) and nally terbuthylazine.
Marketing permission for atrazine and dichlobenil was
withdrawn in Sweden in 1989, whereas terbuthylazine
supersedes atrazine. For analytical identication, the
samples were screened using GC/MS (SIM). The
limits of detection for including pesticides involved
in GC/MS analysis were estimated using standard
solutions. The quantication was made with specic
detectors using two capillary columns.
The method showed a limit of quantication of
0.050.01 mg/l in the method. Detectable concentra-
tions below this level are given as approximative
values, <0.05 or <0.01 mg/l. The pesticides not
detected were reported as not detectable (n.d.). The
data of two procedures were compared by Student's
t-test at 0.05% signicance level. The obtained con-
centrations 0.1 mg/l analysed by the SPE and the
LLE did not give signicantly different values for
involved pesticides, except for desisopropylatrazine,
which was not detected in any samples processed by
the LLE technique. Comparing the SPE method with
the LLE, it is found that the SPE method seems to be
more sensitive by detecting a greater number of
components than the LLE method (Table 6). There
were 63 positive results with SPE and 52 with LLE of
totally 106 samples. The concentrations of the ve
pesticide using the both methods were reasonably
160 T. Pihlstrom et al. / Analytica Chimica Acta 356 (1997) 155163
similar. The measured concentrations obtained with
the SPE were somewhat higher than those with the
LLE. One possible explanation to the improved
extraction efciency is that the SPE is processed
without the evaporation step, which is important for
high volatile pesticides. Maximum concentrations of
BAM, atrazine and desethylatrazine originated from
the same sample (Figs. 14). The measured concen-
trations obtained with the LLE were 2545% of those
analysed with the SPE. Desisopropylatrazine was
detected in three samples in concentrations of
0.1 mg/l, whereas desisopropylatrazine was not found
with LLE (Tables 7 and Table 8). Furthermore, one
Table 6
Number of positive findings in natural waters analysed with SPE
and LLE
Pesticide mg/l
SPE LLE
BAM 16 12
Atrazine 19 18
Desethylatrazine 20 17
Desisopropylatrazine 3 0
Terbuthylazine 5 5
Totally 63 52
Fig. 1. GC/TSD chromatogram of standard solutions of desisopropylatrazine (DIA), desethylatrazine (DEA) and atrazine, 0.03 mg/ml.
Fig. 2. GC/TSD chromatogram of the water sample found to contain residues of DEA and atrazine (diluted 20 times).
Table 7
The occurrence of pesticide residues in ground and surface waters
analysed with SPE and LLE
Pesticide mg/l
SPE LLE
BAM 0.17 <0.1
<0.1 n.d
0.19 0.16
<0.1 n.d.
0.13 <0.1
Atrazine 0.05 <0.05
0.19 0.16
<0.05 <0.05
Desethylatrazine 0.06 <0.05
0.13 0.08
<0.05 n.d.
Terbuthylazine n.d. <0.05
<0.05 n.d.
<0.05 <0.05
<0.05 <0.05
T. Pihlstrom et al. / Analytica Chimica Acta 356 (1997) 155163 161
incurred sample was analysed in triplicate with a
resulting repeatability of 711% (Table 9). Due to
the relatively high detection limits for pyrethroids
with GC/MS screening (Table 2) and the low recov-
eries at 0.05 mg/l, it was difcult to detect any residues
in natural waters. Presumably, an additional concen-
tration step would make it possible to lower the LOD
for screening the pyrethroids.
Fig. 3. GC/MS chromatogram of standard solution containing BAM (Rt 7.5 min) 0.04 mg/ml.
Fig. 4. GC/MS chromatogram of the water sample found to contain BAM (diluted 25 times).
162 T. Pihlstrom et al. / Analytica Chimica Acta 356 (1997) 155163
5. Conclusion
In conclusion, a method for determining a large
number of pesticides with a broad range of polarities
in water has been developed. The obtained concentra-
tions, quantied at the 0.1 mg/l level, which is required
by the E.C. Council Directive for water, indicated that
the results with the SPE is comparable with those from
the LLE. The advantages of this SPE method are its
rapidity and simplicity and that it can be used in the
analysis of large numbers of samples. The method is
also applicable in analysing pesticides in various types
of waters. Factors that may affect recoveries are
elution ow rate, sample loading ow rate and column
drying. In order to control these parameters, automa-
tion of the method would be advantageous in order to
diminish any uncertainty during the analysis.
Acknowledgements
We gratefully acknowledge G. Blomkvist and B.
Hellkvist for sharing their experience and knowledge
in GC/MS methodology. We would like to thank B.
Kajrup and A. Liedgren for their diligence in experi-
mental work in the rst part of the investigation.
References
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[3] M. A

kerblom, L. Thoren, A. Staffas, Var Foda 42 (1990) 236.

[4] D. Rosling, B. Erlandsson, B-G Eriksson, T. Pihlstrom, Var
Foda, 1997, in press.
[5] A. Andersson, T. Bergh, Fresenius J. Anal. Chem. 339 (1991)
387389.
[6] A. Valverde, T. Pihlstrom, A. Andersson, Anal. Chim. Acta
338 (1997) 63.
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Table 8
Analysis of pesticide residues in drinking water using SPE and LLE
Pesticide mg/l
SPE LLE
BAM <0.1 n.d.
<0.1 <0.1
0.12 <0.1
0.15 <0.1
0.16 <0.1
0.22 <0.1
0.28 n.d.
0.40 0.13
0.40 0.11
0.72 0.55
2.44 0.96
Atrazine n.d. <0.05
<0.05 n.d.
<0.05 <0.05
<0.05 <0.05
<0.05 <0.05
<0.05 <0.05
<0.05 <0.05
<0.05 <0.05
0.06 0.06
0.11 0.11
0.12 0.06
0.13 0.15
0.19 0.28
0.30 0.18
0.38 0.26
0.49 0.32
0.89 0.39
Desethylatrazine 0.15 0.07
<0.05 n.d.
<0.05 n.d.
<0.05 <0.05
<0.05 <0.05
<0.05 <0.05
<0.05 <0.05
0.07 0.07
0.09 0.07
0.12 0.06
0.15 0.07
0.20 0.23
0.30 0.12
0.32 0.14
0.38 0.15
0.40 0.15
2.40 0.66
Desisopropylatrazine 0.10 n.d.
0.15 n.d.
0.17 n.d.
Terbuthylazine 0.05 1.00
0.06 <0.05
Table 9
Analysis of a water sample with incurred content. n3
Pesticide Conc. mg/l RSD %
BAM 0.88/0.73/0.73 11
Atrazine 0.28/0.29/0.32 7
Desethylatrazine 0.40/0.39/0.45 8
T. Pihlstrom et al. / Analytica Chimica Acta 356 (1997) 155163 163