Published:Journal of Chromatographic Science,
ISSN 0021-9665 Volume
44, Number 7, August 2006, pp.430-437
Active Sampling Followed by Solid-Phase Microextraction
for the Determination of Pyrethroids in Indoor Air
Ruth Barro, Carmen Garcia-Jares, Maria Llompart,
and Rafael Cela
Departamento de Quimica Analitica, Nutricion y Bromatologia, Facultad
de Quimica, Instituto de Investigacion y Analisis Alimentario,
Universidad de Santiago de Compostela, E-15782 Santiago de Compostela,
Spain
A method based on solid-phase enrichment followed
by headspace (HS)–solid-phase microextraction (SPME) is
optimized to determine pyrethroids in air. By active sampling,
pyrethroids present in air are retained in 25 mg of activated
florisil and then transferred from the solid sorbent to an SPME
fiber in the HS mode. A small volume of solvent is added to the
adsorbent to favor this process. The selection of the adsorbent,
as well as the optimization of certain parameters affecting the
SPME, is performed using an experimental design strategy. Linearity
is studied by external calibration in a wide range of concentrations
using gas chromatography coupled to three different detection
systems: electron capture detection, micro-electron capture detection,
and mass spectrometry. An analysis of variance with a lack-of-fit
test is run to validate the calibration data. Breakthrough of
the adsorbent was studied sampling from 0.5 to 10 m3 air, demonstrating
that 1 m3 air could be sampled without losses of pyrethroids.
Quantitative recoveries are obtained at three concentration levels,
with adequate repeatability. Limits of detection of the method
are estimated at the sub-ng/m3 level in most cases, well below
the regulatory limits. Finally, several real indoor samples are
collected and analyzed by the proposed method. Identification
and quantitation of all target analytes present in the room air
are possible.
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