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Imanol González Burguera

Determination of Fluoxetine and its major active metabolite,
Norfluoxetine, in sewage sludge by HPLC-UV and LC-MS after
Pressurized liquid extraction
One of the key issues in wastewater studies is the emerging problem of micro-
pollutants such as pharmaceutically active contaminants, plastic additives, hormones,
etc. Two interesting pharmaceutical compounds are Fluoxetine and its metabolite
Norfluoxetine. Fluoxetine is a the active ingredient in ProzacTM . These contaminants
normally have low concentrations in water, but it is valuable to know the
environmental fate and the ecological impact of these highly biologically active
compounds.
In this project, a modern extraction technique, Pressurized Liquid Extraction, was
applied to extract these compounds from sewage sludge from the Källby sewage
treatment plant in Lund. The actual determination of the target compounds was made
by liquid chromatography combined with mass spectrometry, which is the most
sensitive and selective techniques available for the purpose. This is a part of a larger
project aiming at studies of the chemical fate of drug residues in the sewage treatment
process.
The result is that the compounds in questions indeed can be found in the sludge from
the sewage treatment plant in concentrations around and below 1 μg/g. The limit of
detection was 0.06 μg/g. This is in agreement with international observations.
Advisor: Jan Åke Jönsson
Degree project 30 credits in Analytical Chemistry 2009
Department of Chemistry., Lund University
Imanol González Burguera

Determination of Fluoxetine and its major active metabolite,
Norfluoxetine, in sewage sludge by HPLC-UV and LC-MS after
Pressurized liquid extraction
In this report, a method has been developed for quantification of fluoxetine and
norfluoxetine, selective serotonin reuptake inhibitors, in the sludge of a wastewater
treatment plant.
The sample preparation has been done by pressurized liquid extraction (PLE), and
concentration in a rotavapor. Before the analysis a cleanup with solid phase extraction
(SPE) by MCX Oasis® cartridge was done. Finally the analysis was carried out by
HPLC/UV to determine that fluoxetine and norfluoxetine appear in the sewage
sludge. To validate their presence another analysis was carried out by LC/MS. With
the HPLC-UV method, we calculate their concentrations, which were 1.3 μg/g for
fluoxetine and 1.4 μg/g for norfluoxetine. Recoveries for both cases were close to
100%.
With LC-MS the results were somewhat lower, probably due to less interference from
other compounds in the sludge: The fluoxetine concentration was 0.2 μg/g and for
norfluoxetine 0.4 μg/g. The limit of detection was 0.06 μg/g. So, with these results we
can say that these two compounds are present in the sewage sludge.
Advisor: Jan Åke Jönsson
Degree project 30 credits in Analytical Chemistry 2009
Department of Chemistry., Lund University

Source: http://it.biol.lu.se/examensarbeten/kemi/090911imgo.pdf

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