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Detection of Pharmaceuticals, Personal Care
Products, and Pesticides in Water Resources by
APCI-LC-MS/MS
Liza Viglino
1
, Khadija Aboulfald
1
, Michèle Prévost
2
, and Sébastien Sauvé
1
1
Department of Chemistry, Université de Montréal, Montréal, QC, Canada;
2
Département of Civil, Geological, and Mining
Engineering, École Polytechnique de Montréal, Montréal, QC, Canada
Introduction
Pharmaceuticals (PhACs), personal care product
compounds (PCPs), and endocrine disruptors (EDCs),
such as pesticides, detected in surface and drinking waters
are an issue of increasing international attention due to
potential environmental impacts
1,2
. These compounds are
distributed widely in surface waters from human and
animal urine, as well as improper disposal, posing a
potential health concern to humans via the consumption
of drinking water. This presents a major challenge to
water treatment facilities.
Collectively referred to as organic wastewater
contaminants (OWCs), the distribution of these emerging
contaminants near sewage treatment plants (STP) is
currently an area of investigation in Canada and
elsewhere
3,4
. More specifically, some of these compounds
have been detected in most effluent-receiving rivers of
Ontario and Québec
5,6
. However, it is not clear whether
contamination is localized to areas a few meters from STP
discharges or whether these compounds are distributed
widely in surface waters, potentially contaminating
sources of drinking water.
A research project at the University of Montreal’s
Chemistry Department and Civil, Geological, and Mining
Engineering Department was undertaken to establish the
occurrence and identify the major sources of these
compounds in drinking water intakes in surface waters in
the Montreal region. The identification and quantification
of PhACs, PCPs, and EDCs is critical to determine the
need for advanced processes such as ozonation and
adsorption in treatment upgrades.
The establishment of occurrence data is challenging
because of: (1) the large number and chemical diversity of
the compounds of interest; (2) the need to quantify low
levels in an organic matrix; and (3) the complexity of
sample concentration techniques. To address these issues,
scientists traditionally use a solid phase extraction (SPE)
method to concentrate the analytes and remove matrix
components.
After extraction, several different analytical techniques
may perform the actual detection such as GC-MS/MS and
more recently, LC-MS/MS
7,8
. Another analytical challenge
resides in the different physicochemical characteristics and
wide polarity range of organic compounds – making
simultaneous preconcentration, chromatography
separation, and determination difficult. Analytical
methods capable of detecting multiple classes of emerging
contaminants would be very useful to any environmental
monitoring program. However, up to now, it has often
been a necessity to employ a combination of multiple
analytical techniques in order to cover a wide range of
trace contaminants
9
. This can add significant costs to
analyses, including equipment, labor, and time
investments.
Goals
To develop a simple method for the simultaneous
determination of trace levels of compounds from a diverse
group of pharmaceuticals, pesticides, and personal care
products using SPE and liquid chromatography-tandem
mass spectrometry (LC-MS/MS).
Determine which selected substances are present in
significant quantities in the water resources around the
Montreal region.
Materials and Method
Analyte selection
Compounds were selected from a list of the most-
frequently encountered OWCs in Canada
4-6
(Figure 1).
Sample collection
Raw water samples were taken from the Mille Iles, des
Prairies, and St-Laurent rivers. Three samples were
collected at the same time from each river in pre-cleaned,
four-liter glass bottles and kept on ice while being
transported to the laboratory. These water sources vary
widely due to wastewater contamination and sewer
overflow discharges.
All samples were acidified with H
2
SO
4
for sample
preservation and stored in the dark at 4 °C. Immediately
before analysis, samples were filtered using 0.7 µm pore-
size fiberglass filters followed by 0.45 µm pore size mixed-
cellulose membranes (Millipore, MA, USA). Samples were
extracted within 24 hours of collection.
Key Words
• TSQ Quantum
Ultra
• Water Analysis
• Solid Phase
Extraction
Application
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