Talanta 82 (2010) 1864–1869
Contents lists available at ScienceDirect
Talanta
journal homepage: www.elsevier.com/locate/talanta
Application of surfactant assisted dispersive liquid–liquid microextraction for
sample preparation of chlorophenols in water samples
Morteza Moradi, Yadollah Yamini
∗
, Ali Esrafili, Shahram Seidi
Department of Chemistry, Faculty of Sciences, Tarbiat Modares University, P.O. Box 14115-175, Tehran, Iran
article info
Article history:
Received 10 June 2010
Received in revised form 31 July 2010
Accepted 3 August 2010
Available online 10 August 2010
Keywords:
Surfactant assisted dispersive liquid–liquid
microextraction
Chlorophenols
Natural water samples
High performance liquid chromatography
abstract
A simple, rapid, and efficient method, based on surfactant assisted dispersive liquid–liquid microextrac-
tion (SA-DLLME), followed by high performance liquid chromatography (HPLC) has been developed for
the extraction and determination of chlorophenols as model compounds in environmental water sam-
ples. A conventional cationic surfactant called cethyltrimethyl ammonium bromide (CTAB) was used as
a disperser agent in the proposed approach. Thirty-five microliter of 1-octanol as an extraction solvent
was injected rapidly into 11 mL aqueous sample containing 0.09 mmol L
-1
of CTAB, the mixture was then
shaken for 3 min to disperse the organic phase. Having the extraction procedure been completed, the
mixture was centrifuged and 20 L of collected phase was injected into HPLC for subsequent analysis.
Some parameters such as the type and volume of the extraction solvent, the type and concentration
of surfactant, pH, ionic strength, shaking time, extraction temperature and centrifugation time were
optimized. The preconcentration factors (PFs) in a range of 187–353 were obtained under the optimum
conditions. The linear range, detection limit (S/N = 3), and precision (n = 5) were 0.2–200, 0.1 gL
-1
, and
4.7–6.9%, respectively. Tap water, sea water and mineral water samples were successfully analyzed for
the existence of chlorophenols using the proposed method.
© 2010 Elsevier B.V. All rights reserved.
1. Introduction
Phenol and substituted phenols are widely distributed in natural
waters because of their wide use in many industrial processes such
as the manufacture of plastics, dyes, drugs and pesticides [1–3].
Among these compounds, chlorophenols are well known pollutants
because of their toxicity in aquatic life and poor biotreatability, and
since they make an unpleasant taste and odor in water even in
very low concentrations. Chlorophenols are formed by the degra-
dation of phenoxy herbicides, as well as by the chlorination of
drinking water containing aromatic impurities [4–6]. The European
Community legislation has also set a maximum allowable phe-
nol concentration of 0.5 gL
-1
in tap water [7]. The importance
of chlorophenols in environment, calls for sensitive and reliable
methods to determinate them in water samples. Many methods
for analysis of chlorophenols are based on chromatographic tech-
niques such as high performance liquid chromatography (HPLC)
[8–10], gas chromatography (GC) [11–13] and capillary elec-
trophoresis [14,15]. The GC analysis of the chlorophenols leads to
tailed peaks resulting decreasing the detection limits and the reli-
ability of the results. To alleviate this drawback, chlorophenols are
usually derivatized with a suitable derivatization reagent before
∗
Corresponding author. Tel.: +98 21 82883417; fax: +98 21 88006544.
E-mail address: yyamini@modares.ac.ir (Y. Yamini).
injection into the GC. On the other hand, HPLC is a good alterna-
tive technique, in which isocratic or gradient elution can be used
to separate the compounds.
In general, the environmental samples are too diluted or too
complex. Therefore, prior to analysis by HPLC, a sample prepa-
ration step is necessary to extract traces of chlorophenols from
the aqueous medium, bring the analytes to a suitable concentra-
tion level, and remove them from interfering components in the
matrix [16]. Typically, this would require an extraction step such as
liquid–liquid extraction (LLE) or solid phase extraction (SPE). How-
ever, conventional LLE consumes large amounts of the high costing
and potentially hazardous organic solvents. In addition, in trace
analysis, a large volume of sample is often required and its handling
can be extremely time consuming besides being tedious. SPE uses
much less solvent and is less time consuming than LLE but requires
column conditioning and is relatively expensive [17]. The first
attempts to miniaturize the conventional LLE have been developed
by Liu and Dasgupta [18,19] and Jeannot and Cantwell [20]. The
first suggested method of liquid phase microextraction (LPME) was
a single drop microextraction (SDME). This technique is performed
by suspending a microliter drop of organic solvent in the stirred
aqueous solution, in which the analytes are partitioned between
the organic drop and the aqueous phase. Several different types of
LPME methods have been developed, including hollow fiber LPME
[21], homogeneous liquid–liquid extraction (HLLE) [22,23] and
solidification of a floating organic drop (SFO) [24]. Microextraction
0039-9140/$ – see front matter © 2010 Elsevier B.V. All rights reserved.
doi:10.1016/j.talanta.2010.08.002