Published:Journal of Chromatographic Science,
ISSN 0021-9665 Volume 44,
Number 7, August 2006, pp. 458
Trace Element Determination by Combining Solid-Phase
Microextraction Hyphenated to Elemental and Molecular Detection
Techniques
Sergi Díez and Josep M. Bayona
Environmental Chemistry Department, IIQAB-CSIC, Jordi Girona,
18–26, 08034 Barcelona, Spain
The state of the art of analytical procedures based
on solid-phase microextraction (SPME) and its applications to
tin, mercury, arsenic, antimony, chromium, selenium, and lead
determination in abiotic and biotic matrixes are critically reviewed
from 1994 to present. First, sample pretreatment prior to SPME
is evaluated, including a description of the most usual leaching
procedures for sediment, soil, and biological samples. Because
most organometallic species lack volatility, a derivatization
step is mandatory prior to gas chromatographic (GC) determination,
except for the volatile organometallics that can be directly extracted
from the sample headspace or liquid phase by SPME. The most common
derivatization procedures used in alkylation and hydridization
reactions used for mercury, lead, and tin, as well as other procedures
for the determination of total chromium and arsenic [i.e., trifluoroacetylacetonates
for chromium (III) and thioglycol methylate for organic arsenic
species] are reviewed. Critical variables usually evaluated along
with the method development to improve the sensitivity of the
extraction methods based on SPME, such as sampling size, stirring
procedures, sampling temperature and pressure, polymer coating,
and thermal desorption are reviewed. In addition, figures of merit
of the different detection systems used in SPME combined with
GC are evaluated. The validation of the reported analytical procedures
with reference materials are also discussed in terms of precision
and accuracy. Finally, future developments in the application
of SPME to speciation are highlighted. Moreover, the capability
of SPME automation for the derivatization–extraction procedures
are also presented.
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