Environmentally friendly analysis of emerging contaminants by pressurized hot water extraction-stir bar sorptive extraction-derivatization and gas chromatography-mass spectrometry

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URI: http://hdl.handle.net/10498/17233
DOI: 10.1007/s00216-012-6453-1
URL: http://link.springer.com/article/10.1007%2Fs00216-012-6453-1
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2013-01-01Department
Química FísicaSource
Analytical and Bioanalytical Chemistry January 2013, Volume 405, Issue 1, pp 401-411Abstract
This work describes the development, optimiza-
tion, and validation of a new method for the simultaneous
determination of a wide range of pharmaceuticals (beta-
blockers, lipid regulators
...
) and personal care products
(fragrances, UV filters, phthalates
...
) in both aqueous and
solid environmental matrices. Target compounds were
extracted from sediments using pressurized hot water ex-
traction followed by stir bar sorptive extraction. The first
stage was performed at 1,500 psi during three static extrac-
tion cycles of 5 min each after optimizing the extraction
temperature (50
–
150 °C) and addition of organic modifiers
(% methanol) to water, the extraction solvent. Next, aqueous
extracts and water samples were processed using polydime-
thylsiloxane bars. Several parameters were optimized for
this technique, including extraction and desorption time,
ionic strength, presence of organic modifiers, and pH. Fi-
nally, analytes were extracted from the bars by ultrasonic
irradiation using a reduced amount of solvent (0.2 mL) prior
to derivatization and gas chromatography
–
mass spectrome-
try analysis. The optimized protocol uses minimal amounts
of organic solvents (<10 mL/sample) and time (
≈
8 h/sam-
ple) compared to previous ex
isting methodologies. Low
standard deviation (usually below 10 %) and limits of de-
tection (sub-ppb) vouch for the applicability of the method-
ology for the analysis of target compounds at trace levels.
Once developed, the method was applied to determine
Subjects
extraction; emerging compounds; GC-MSCollections
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