Loading...
Publication
Development of new analytical methods for the analysis of an emerging pharmaceutical pollutant (ibuprofen): analysis by capillary electrophoresis and HPLC coupled with off-line SPE
| Name: | Description: | Size: | Format: | |
|---|---|---|---|---|
| 3.14 MB | Adobe PDF |
Authors
Advisor(s)
Abstract(s)
Pharmaceuticals have become priority emerging environmental pollutants.
Environmental monitoring and toxicological studies are essential to establish maximum
permissible limits in the environment. Furthermore, innovative wastewater treatment is
required for their degradation. Águas do Algarve is constructing an aerobic granule plant to
modernize wastewater treatment for the cities of Faro and Olhão. The company is interested in
research regarding granule ability to degrade pharmaceuticals detected in wastewater influent.
Two aerobic granule sequencing batch reactors were constructed and operated at
laboratory scale using different cycles (anaerobic/aerobic and aerobic). The efficiency of the
reactors and type of operating conditions was investigated for the degradation and removal of
ibuprofen and its metabolites 2-hydroxyibuprofen, 1-hydroxyibuprofen and carboxyibuprofen.
Two methods, high performance liquid chromatography (HPLC) and micellar
electrokinetic chromatography (MEKC), a form of capillary electrophoresis, coupled with
UV/Vis, were developed to detect and quantify ibuprofen and its metabolites. Solid phase
extraction was used to preconcentrate the compounds to method detection limits, however
recoveries were problematic. Eluents were dried and reconstituted in solvent (milli-q water)
for compatibility to both methods. Separation conditions for the compounds were optimized.
Both methods were validated in solvent (milli-q water) for linearity, recovery, LOD, LOQ,
precision (repeatability and intermediate precision), range and selectivity. Selectivity could be
obtained for both methods. However, acceptable linearity, LOD, LOQ, repeatability and
recovery could not be established in the desired working range. Additionally, robustness
problems particularly for the MEKC method may have affected validation results. For some
compounds, both methods failed to meet statistical tests applied for acceptance of linearity and
repeatability. Solvent and synthetic wastewater calibration were compared using student’s ttest.
There was no statistically significant difference between the curves for the HPLC method
in contrast to those of the MEKC method.
The methods were applied to synthetic wastewater samples taken from the SBRs. Each
method detected different analytes with 1-hydroxyibuprofen observed in HPLC and
carboxyibuprofen observed in MEKC. The calculated concentrations exceeded method range.
Revalidation of both methods and reanalysis of the samples is required to verify accuracy of
results and confirm suitability for intended application.
Description
Dissertação de mestrado, Qualidade em Análises, Faculdade de Ciências e Tecnologia, Universidade do Algarve, 2017
Keywords
High performance liquid chromatography Micellar electro kinetic chromatography Capillary electrophoresis Ibuprofen Metabolites Validation Wastewater Aerobic granule