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.

[1]  Heinrich Hühnerfuss,et al.  Results of non target screening of lipophilic organic pollutants in the German Bight II : Polycyclic musk fragrances , 1998 .

[2]  Martin Schlabach,et al.  Gas chromatographic determination of synthetic musk compounds in Norwegian air samples , 1999 .

[3]  M. Winkler,et al.  Optimization of solid-phase microextraction for the gas chromatographic-mass spectrometric determination of synthetic musk fragrances in water samples. , 2000, Journal of chromatography. A.

[4]  R. Draisci,et al.  Evaluation of musk contamination of freshwater fish in Italy by accelerated solvent extraction and gas chromatography with mass spectrometric detection. , 1998, Journal of chromatography. A.

[5]  R. Cela,et al.  Determination of phenols in soils by in situ acetylation headspace solid‐phase microextraction , 2000 .

[6]  Janusz Pawliszyn,et al.  Solid phase microextraction : theory and practice , 1997 .

[7]  T. Heberer,et al.  Occurrence and Distribution of Organic Contaminants in the Aquatic System in Berlin. Part III: Determination of Synthetic Musks in Berlin Surface Water Applying Solid-phase Microextraction (SPME) and Gas Chromatography-Mass Spectrometry (GC-MS) , 1999 .

[8]  V Berding,et al.  Aquatic fate assessment of the polycyclic musk fragrance HHCB. Scenario and variability analysis in accordance with the EU risk assessment guidelines. , 2000, Chemosphere.

[9]  G. Rimkus,et al.  Nitro musk fragrances in biota from freshwater and marine environment , 1995 .

[10]  T. Ternes,et al.  Pharmaceuticals and personal care products in the environment: agents of subtle change? , 1999, Environmental health perspectives.

[11]  C. Struppe,et al.  Nitro musks in cosmetic products—determination by headspace solid-phase microextraction and gas chromatography with atomic-emission detection , 1997 .

[12]  J. Pawliszyn,et al.  Determination of phenols by solid-phase microextraction and gas chromatographic analysis , 1993 .

[13]  H. H. Wisneski.  Determination of musk ambrette, musk xylol, and musk ketone in fragrance products by capillary gas chromatography with electron capture detection. , 2001, Journal of AOAC International.