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Anal Bioanal Chem. 2009 Jul;394(5):1399-411. doi: 10.1007/s00216-009-2829-2. Epub 2009 May 21.

Solid-phase microextraction gas chromatography-mass spectrometry determination of fragrance allergens in baby bathwater.

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Departamento de Quimica Analitica, Nutricion y Bromatologia, Facultad de Quimica, Instituto de Investigacion y Analisis Alimentario, Campus Sur, Universidad de Santiago de Compostela, 1578 Santiago de Compostela, Spain.


A method based on solid-phase microextraction (SPME) and gas chromatography-mass spectrometry (GC-MS) has been optimized for the determination of fragrance allergens in water samples. This is the first study devoted to this family of cosmetic ingredients performed by SPME. The influence of parameters such as fibre coating, extraction and desorption temperatures, salting-out effect and sampling mode on the extraction efficiency has been studied by means of a mixed-level factorial design, which allowed the study of the main effects as well as two-factor interactions. Excluding desorption temperature, the other parameters were, in general, very important for the achievement of high response. The final procedure was based on headspace sampling at 100 degrees C, using polydimethylsiloxane/divinylbenzene fibres. The method showed good linearity and precision for all compounds, with detection limits ranging from 0.001 to 0.3 ng mL(-1). Reliability was demonstrated through the evaluation of the recoveries in different real water samples, including baby bathwater and swimming pool water. The absence of matrix effects allowed the use of external standard calibration to quantify the target compounds in the samples. The proposed procedure was applied to the determination of allergens in several real samples. All the target compounds were found in the samples, and, in some cases, at quite high concentrations. The presence and the levels of these chemicals in baby bathwater should be a matter of concern.

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