Optimisation of a solid-phase microextraction method for synthetic musk compounds in water.
A solid-phase microextraction method (SPME) for determining trace levels of synthetic musk fragrances in residual waters has been developed. Six polycyclic musks (cashmeran, phantolide, celestolide, traseolide, galaxolide and tonalide), and a macrocyclic musk (ambrettolide) have been analysed. A detailed study of the different parameters affecting the extraction process is presented. The main important factors affecting the microextraction process have been studied and optimised by means of a categorical factorial design. Two extraction modes (direct SPME and headspace SPME) were tried at different extraction temperatures using four different fiber coatings [polydimethylsiloxane (PDMS), Carboxen (CAR)-PDMS, PDMS-divinylbenzene (DVB) and Carbowax (CW)-DVB]. An extraction temperature of 100 degrees C sampling the headspace over the sample using CAR-PDMS or PDMS-DVB as fiber coatings were found to be the experimental conditions that lead to a more effective extraction. The method proposed is very simple and yields high sensitivity, with detection limits in the low pg/ml, good linearity and repeatability for all the target compounds. The total analysis time, including extraction and GC analysis, was only 45 min. The optimised method performed well when it was applied to waste water from an urban treatment plant.
García-Jares
Carmen
C
Departamento de Química Analítica, Nutrición y Bromatología, Facultad de Química, Universidad de Santiago de Compostela, Spain. qncgj@usc.es
Llompart
Maria
M
Polo
María
M
Salgado
Carmen
C
Macías
Susana
S
Cela
Rafael
R
D005229:Fatty Acids, Monounsaturated / Q000032:analysis*; D008401:Gas Chromatography-Mass Spectrometry / Q000379:methods*; D015203:Reproducibility of Results; D012680:Sensitivity and Specificity; D014874:Water Pollutants, Chemical / Q000032:analysis*
D005229:Fatty Acids, Monounsaturated; D014874:Water Pollutants, Chemical; C008563:musk