Journal of Analytical & Bioanalytical Techniques
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Qualitative and quantitative analysis usually includes a sample preparation procedures,
which today are still the weakest link and the time-determining step in the whole
analytical method. However, due to the complex nature of the matrices and the low
detection levels required by regulations, an effi
cient sample preparation is an important
aspect of analytical methods. Th
is step is basically the most time-consuming part of
an analysis, therefore, various attempts have been made to replace classical extraction
techniques (leaching by mechanical shaking, ultrasound extraction, microwave-assisted
extraction, supercritical fl
uid extraction) in order to short the sample preparation time
and simplify the procedure.
Although Pressurised Liquid Extraction (PLE) has been designed and used mainly
for organic compounds extraction, in recent years it has been successfully applied for
extracting organometallic species. PLE is based on the use of solvents at a high pressure
and/or high temperature without reaching the critical point, which improves effi
over classical extractions by shortening extractions times and reducing solvent volumes.
e usefulness of PLE for total metal extraction from biological (GBW-08751 mussel tissue,
sh muscle, DOLT-3 dog-fi
sh liver, TORT-2 lobster hepatopancreas, GBW-
07601 human hair, NIEST-03
), inorganic (PACS-2
marine sediment, GBW-0709 soil, IRANT-12-1-07 cambisol soil, IRANT-12-1-08 luvisol
soil) and atmospheric particulate matter samples have been tested. Th
e suitability of
erent carboxylic acids (acetic acid, formic acid, oxalic acid, citric acid and ascorbic
acid) and chelating solvents (EDTA, PHEN, 8HQ, CT, AMPAHC and DFC) as solvents
for PLE, have been assayed to extract metals. Inductively Coupled Plasma ? Optical
Emission Spectrometry (ICP-OES) has been used for the multi?element determination.
Variables inherent to PLE (temperature, solvent concentration, static time, pressure,
number of cycles, dispersing agent mass, fl
ush volume and purge time) were simultaneously
studied and optimised by applying an experimental design approach (Plackett?Burman
design, PBD, and central composite design, CCD).
High metal recoveries and short extraction times (when comparing to conventional
sample pre-treatments) obtained, avoiding of extract handling (a fi
ltration step is not
required) and use of less toxic reagents/acids at low concentrations (environmental
friendly procedures), allow to conclude that PLE can be a real, practical and promising
procedure for total metal extraction from environmental samples.
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