Download Nome Completo: Ana Valéria Colnaghi Simionato

Sociedade Brasileira de Espectrometria de Massas – BrMASS
GC/LC
Determination of pharmaceutical drugs in tap and river water
using solid phase microextraction-comprehensive two
dimensional gas chromatography-time of flight mass
spectrometry (SPME-GCxGC-ToF/MS)
Paulo C. F. L. Gomes*1,2, Brian Barnes2, Álvaro J. Santos-Neto1, Fernando M. Lancas1,
Nicholas H. Snow2
[email protected]
Institute of Chemistry of Sao Carlos, University of Sao Paulo, Postal Code 780, 13560970 São Carlos, SP, Brazil
2
Department of Chemistry and Biochemistry, Center for Academic Industry Partnership,
Seton Hall University, 400 South Orange Avenue, South Orange, NJ, 07079, USA
1
Pharmaceutical residues have been detected in the environment as a
consequence of their widespread usage in hospitals, industries, agriculture, livestock
and household. However, these drug residues usually occur at low concentration (ng L1
) in the environment. Therefore, mass spectrometric (MS) detection, due to its
selectivity and sensitivity, is an essential tool for identifying and quantifying the
presence of these pollutants (1). Indeed, hyphenated MS techniques, as gas
chromatography (GC) and comprehensive two dimensional gas chromatography
(GCxGC), are powerful tools in environmental analysis. Nevertheless, before its
introduction into GC, the sample should be submitted to a sample preparation process.
Solid phase microextraction (SPME) is a solventless sample preparation technique that
integrates sampling, extraction and concentration in one single stage. This study
presents the development of a procedure, which enables the analysis of thirteen
pharmaceutical drugs in water by GCxGC-ToF/MS. SPME was used in the sample
preparation procedure and experimental design was applied to optimize this step. A
fractional factorial design evaluated primarily the main factors related to the SPME
extraction. Thereafter, Doehlert matrix design was used to find out the best SPME
extraction conditions. The SPME-GCxGC-ToF/MS method presented a linear range from
0.6 to 1200 µg L-1, where the intra-day and inter-day precision were lower than 14%.
The limit of detection and quantification varied from 0.02 to 100 µg L-1. A series of
river water samples were subjected to analysis and none of the compounds were
present at the detectable levels.
[1] Radjenovic, J.; Petrovic, M.; Barceló, D. Anal. and Bioanal. Chem. 2007, 387, 1365-1377.
4º Congresso BrMass – 10 a 13 de Dezembro de 2011