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Analysis of Pesticide Residues in Soil. New Approaches for Environmental Monitoring
Publication . Brinco, João Eduardo Rodrigues Sedas; Guedes, Paula; Ribeiro, Alexandra; Silva, Marco
Environmental monitoring is a very important part of dealing with soil contamination
problems. As an essential support for life on land, soil should be protected and monitored.
This dissertation is centered on the development of methodologies for pesticide residues
analysis in soil, which are of great relevance due to being widely applied on agricultural
soils and by having known detrimental effects.
The first work presented comprises a method development and monitoring campaign
of empty pesticide packaging from Portugal in order to determine their hazardousness.
The compounds most found in this monitoring along with those frequently reported in the
relevant literature as being present in European Union (EU) soils were used to construct a
list of priority analytes to focus on. This list contained thirteen currently used pesticides
and one degradation product; of these, the herbicide glyphosate is the most challenging
in analytical terms.
A literature review on currently used methods for pesticide residue analysis in soil
was conducted, along with a side-by-side comparison of their properties. QuEChERS
was found to be the most widely used and promising extraction method currently em-
ployed. However, none of the methodologies studied seemed particularly fitted to extract
"multiclass" pesticides along with glyphosate, and thus a new form of extraction using
semi-disposable Solid-Phase Microextraction (SPME) fibers on an aqueous soil slurry was
developed, and combined with solid-liquid extraction followed by chemical derivatization
in order to permit this analysis in a single run employing Gas Chromatography coupled
to tandem Mass Spectrometry (GC-MS/MS).
The same semi-disposable SPME fibers were also applied to the development of a new
"on-the-fly" detection method for pesticides in soil which forgoes traditional sampling
and extensive lab-work. The fibers are inserted directly into the soil, after which they are
retro-extracted onto a suitable solvent and analysed through GC-MS/MS. The proposed
method was tested for monitoring on an electrokinetic remediation experiment at the lab
scale. Results show that this new methodology cannot be used for accurate quantification,
but may be employed in qualitative analysis for detection of contaminants above a certain
confidence threshold.Throughout the work different pieces of software were written in the Python language
to perform calculations, mostly for experimental design and quantification/validation.
These were compiled and documented in a package called Chromapy, which is now freely
available for use and modification.
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Fundação para a Ciência e a Tecnologia
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OE
Número da atribuição
UI/BD/150867/2021