Analytica Chimica Acta 445 (2001) 29–34
Determination of triazine herbicides by capillary liquid
chromatography with on-column focusing and
temperature gradient
M.E. León-González
a,∗
, L.V. Pérez-Arribas
a
, L.M. Polo D´ ıez
a
,
C. Panis
b
, M.P. San Andrés
c
a
Departmento de Qu´ ımica Anal´ ıtica, Facultad de Ciencias Qu´ ımicas, Universidad Complutense, E-28040 Madrid, Spain
b
Engineer’s School CPE, 69616 Lyon, France
c
Departmento de Qu´ ımica Anal´ ıtica, Facultad de Ciencias, Universidad de Alcalá, 28871 Alcalá de Henares, Madrid, Spain
Received 20 March 2001; received in revised form 11 June 2001; accepted 29 June 2001
Abstract
The combination of capillary liquid chromatography, temperature gradient and on-column focusing with large injection
volumes offers a powerful tool for the determination of very low concentrations of triazines and their degradation products
when very polar degradation products are present. A temperature gradient from subambient temperatures up to 70
◦
C allows
separation of eight triazines in 24 min. The focusing step makes it possible to increase 50 times the sample volume that can
be injected into a capillary column. Detection limits (3 × noise) are improved by a factor between 50 and 125 to 9 ng l
-1
for
hydroxyatrazine and 45 ng l
-1
for atrazine. The chromatographic method, combined with solid phase extraction, was applied
to the determination of eight triazines in ground water. © 2001 Elsevier Science B.V. All rights reserved.
Keywords: Capillary liquid chromatography; Temperature programming; Column focusing; Triazine herbicides; Water
1. Introduction
The extensive use of chlorotriazines as selective
herbicides in agriculture and their relatively high per-
sistence imply that these compounds could now be
present in water, soil and food. In the European coun-
tries, the maximum admissible amount of these in-
dividual herbicides should not exceed 0.1 gl
-1
in
drinking water, and the alert or alarm threshold values
should be 1 or 3 gl
-1
, respectively, in surface water
∗
Corresponding author. Tel.: +34-913944331;
fax: +34-913944329.
E-mail address: leongon@eucmax.sim.ucm.es
(M.E. Le´ on-Gonz´ alez).
[1]. Triazines can also be altered by physical, chemi-
cal and biological processes into one or more degra-
dation products, some of which can be more toxic or
persistent than the parent compound [2]. Hence, there
is a need for analytical procedures for monitoring pes-
ticides and their transformation products in environ-
mental matrices.
Triazines have been determined using a variety
of techniques, including gas chromatography (GC)
with selective detection [3–6], liquid chromatogra-
phy (LC) [2,7–11] and a combination of these tech-
niques with mass spectrometry (MS) [2,4,12–16].
Although GC allows triazines determination, when
thermolabile components of the group, such as metho-
protryn, or very polar metabolites are present, LC
0003-2670/01/$ – see front matter © 2001 Elsevier Science B.V. All rights reserved.
PII:S0003-2670(01)01243-0