Journal of Chromatography A, 1101 (2006) 179–184
Analysis of phenols in water by high-performance liquid chromatography
using coumarin-6-sulfonyl chloride as a fluorogenic precolumn label
Fakhr Eldin O. Suliman
∗
, Suad S. Al-Kindi, Salma M.Z. Al-Kindy, Haider A.J. Al-Lawati
Sultan Qaboos University, College of Science, Box 36, Department of Chemistry, Al-Khod 123, Oman
Received 23 June 2005; received in revised form 25 September 2005; accepted 29 September 2005
Available online 2 November 2005
Abstract
A simple, sensitive and rapid reversed-phase high-performance liquid chromatography (RP-HPLC) method is proposed for the analysis of
some environmentally important phenols in water. The use of coumarin-6-sulphonyl chloride (C6SCl) as a fluorescence-labeling reagent has been
investigated. The compound reacts with phenols within 20 min under mild conditions (ambient temperature, pH 9.0) to give sulphonates that can be
separated by RP-HPLC employing fluorescence detection at λ
ex
= 360 and λ
em
= 460 nm. The optimum conditions for fluorescence, derivatization
and chromatographic separation have been established and detection limits in the range 0.1–0.9 gl
-1
were obtained for the studied compounds. The
calibration curves were linear for the range 6–200 gl
-1
for phenol, 3–200 gl
-1
for 2-chlorophenol, 4-chlorophenol and 2,3,5-trichlorophenol and
for the range of 3–100 gl
-1
for 2,3-dichlorophenol and 3,5-dichlorophenol. The practical applicability of the method to environmental samples
was demonstrated by analyzing drinking and industrial water samples spiked with the phenolic compounds.
© 2005 Elsevier B.V. All rights reserved.
Keywords: Phenols; HPLC; Fluorescence; Cuomarin-6-sulfonyl chloride
1. Introduction
There is a growing concern regarding the quality of water
especially in regions suffering from water shortage. Among
various water pollutants, phenol and substituted phenols are con-
sidered toxic and may cause various problems [1]. Phenol is used
to prepare aspirin and dyes, and most of it is converted to pheno-
lic resins used in adhesives and plastics [2,3]. They are used as
antiseptics, in pharmaceutical products, cosmetics and in a wide
range of agricultural and industrial processes [4–7]. Chlorophe-
nols, such as 2-chlorophenol (2-CP), 2,4-dichlorophenol (2,4-
DCP) and 2,4,6-trichlorophenol (2,4,6-TCP), are known to be
present in water following disinfection processes [8]. They find
their way to rivers water, ground water, wastewater, sediments
and soil as a result of their wide use.
Generally, toxic phenols include chloro-, bromo-, nitro-, and
alkylphenols. Some of these compounds are either known or
suspected endocrine disruptors or carcinogens [9–11]. They are
lipophilic in nature and are readily capable of interfering with the
∗
Corresponding author.
E-mail address: fsuliman@squ.edu.om (F.E.O. Suliman).
cell respiration system [12]. The carcinogenicity of chlorophe-
nols is still controversial; nevertheless a significant increase in
soft-tissue sarcomas and non-Hodgkin’s lymphomas has been
linked to the presence of chlorophenols [13].
Owing to their toxicity, presence in the environment and their
unpleasant organoleptic properties, phenols have been added to
the priority lists of pollutants by the United States Environmental
Protection Agency (EPA), and by the European Union (EU)
[14–16]. The standard permissible level of total phenols is stated
to be 0.5 gl
-1
in drinking water, however, concentration of
individual phenols must not exceed 0.1 gl
-1
.
A great deal of emphasis is placed on the development
of effective, sensitive and reliable analytical methods with an
improved recovery for monitoring trace levels of various phe-
nols in water. This is envisaged by the rapidly growing concern
about the quality of water, and the toxicity brought about by
a number of contaminants including phenols. The early most
popular methods for the determination of phenols are based on
the reaction with 4-aminoantipyrine (4-AAP) in alkaline media
[17,18]. In addition various methods for the assay of phenols
have been reported employing gas chromatography, liquid chro-
matography and capillary electrophoresis with various modes
of detection, such as fluorimetry, spectrometry, chemilumines-
0021-9673/$ – see front matter © 2005 Elsevier B.V. All rights reserved.
doi:10.1016/j.chroma.2005.09.094