Journal of Chromatography A, 1216 (2009) 5895–5902
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Journal of Chromatography A
journal homepage: www.elsevier.com/locate/chroma
Determination of selected UV filters in indoor dust by matrix solid-phase
dispersion and gas chromatography–tandem mass spectrometry
N. Negreira, I. Rodríguez
∗
, E. Rubí, R. Cela
Departamento de Química Analítica, Nutrición y Bromatología, Instituto de Investigación y Análisis Alimentario, Universidad de Santiago de Compostela,
Santiago de Compostela 15782, Spain
article info
Article history:
Received 27 March 2009
Received in revised form 26 May 2009
Accepted 5 June 2009
Available online 10 June 2009
Keywords:
UV filters
Dust
Indoor atmospheres
Matrix solid-phase dispersion
Gas chromatography–tandem mass
spectrometry
abstract
A simple, inexpensive sample preparation procedure, based on the matrix solid-phase disper-
sion (MSPD) technique, for the determination of six UV filters: 2-ethylhexyl salicylate (EHS),
3,3,5-trimethylcyclohexyl salicylate (Homosalate, HMS), 3-(4-methylbenzylidene) camphor (4-MBC),
isoamyl-p-methoxycinnamate (IAMC), 2-ethylhexyl-p-methoxycinnamate (EHMC) and octocrylene
(OCR), in dust from indoor environments is presented and the influence of several operational parameters
on the extraction performance discussed. Under the final working conditions, sieved samples (0.5 g) were
mixed with the same amount of anhydrous sodium sulphate and dispersed with 2 g of octadecyl bonded
silica (C18) in a mortar with a pestle. This blend was transferred to a polypropylene solid-phase extraction
cartridge containing 2 g of activated silica, as the clean-up co-sorbent. The cartridge was first rinsed with
5 mL of n-hexane and the analytes were then recovered with 4 mL of acetonitrile. This extract was adjusted
to 1mL, filtered and the compounds were determined by gas chromatography combined with tandem
mass spectrometry (GC–MS/MS). Recoveries for samples spiked at two different concentrations ranged
between 77% and 99%, and the limits of quantification (LOQs) of the method between 10 and 40 ng g
-1
.
Analysis of settled dust from different indoor areas, including private flats, public buildings and vehicle
cabins, showed that EHMC and OCR were ubiquitous in this matrix, with maximum concentrations of
15 and 41 gg
-1
, respectively. Both UV filters were also quantified in dust reference material SRM 2585
for first time. EHS, 4-MBC and IAMC were detected in some of the analyzed samples, although at lower
concentrations than EHMC and OCR.
© 2009 Elsevier B.V. All rights reserved.
1. Introduction
UV filters are compounds designed to mitigate the deleterious
effects of sunlight. Most of them are organic substances, character-
ized by single or multiple aromatic structures, often with attached
hydrophobic groups [1]. One of their most common uses is in sun-
screens, which are preparations that are applied directly on the
skin to protect against UV radiation. Many countries have legis-
lated both maximum allowable concentrations of UV filters and
the combination of individual organic compounds that can be
included in these products. For example, in the European Union,
26 organic compounds have been approved to be incorporated
in sunscreens at individual concentrations up to 10%, for most of
them [2,3]. Moreover, they are also included in the formulation
of other personal care products (cosmetics, hair dyes and sham-
poos) and used in the protection of goods, plastics, varnishes and
clothes [4–7]; however, no data could be traced related to the type
∗
Corresponding author. Tel.: +34 981 563100x14387; fax: +34 981 595012.
E-mail address: isaac.rodriguez@usc.es (I. Rodríguez).
of UV absorbers and the concentrations incorporated in these mate-
rials.
As many other daily usage compounds, UV filters are continu-
ously discharged into the aquatic environment. Washing off from
the skin, during bathing and swimming, and indirect releases from
towels and clothes contribute significantly to their presence in
surface and wastewater samples [8]. The behaviour of these com-
pounds in the aquatic environment depends on a number of factors
such as (1) their stability during wastewater treatments [4,9,10], (2)
their physicochemical properties, particularly their water solubil-
ity, and (3) their potential transformation through photochemical
and/or oxidation reactions [11,12]. Medium and highly polar UV
filters, such as 2-hydroxy-4-methoxybenzophenone (BP-3) and 2-
hydroxy-4-methoxybenzophenone-5-sulphonic acid (BP-4) have
been often detected in surface and wastewater [6,7,13]; moreover,
BP-4 is not effectively removed by conventional sewage treatments
[6]. More lipophilic species, such as 3-(4-methylbenzylidene)
camphor (4-MBC), 2-ethylhexyl-p-methoxycinnamate (EHMC) and
octocrylene (OCR) have been found in river and lake sediments [14],
sludge [15] and even in biota [4,16]. In fact, concentrations of up to
2 gg
-1
have been reported for 4-MBC and OCR in fish [16] and as
0021-9673/$ – see front matter © 2009 Elsevier B.V. All rights reserved.
doi:10.1016/j.chroma.2009.06.020