Pressurized liquid extraction with in-cell clean-up followed by gas chromatography-tandem mass spectrometry for the selective determination of parabens and triclosan in indoor dust.
A sample preparation method based on the use of pressurized liquid extraction is proposed for the determination of four alkyl parabens and triclosan in indoor dust. Extraction of analytes and removal of interfering species were achieved in the same step, by placing an appropriate sorbent in the extraction cell and by choosing a right combination of washing and elution solvents. Compounds, as silylated derivatives, were determined by gas chromatography in combination with tandem mass spectrometry (GC-MS/MS). Factors affecting the yield and selectivity of the sample preparation procedure were carefully evaluated. Under final conditions, dried samples (0.5 g of dust and 1g of sodium sulphate) were dispersed with 3g of Florisil and loaded into an 11 mL stainless-steel extraction cell containing 1g of the same material as clean-up sorbent. Non-polar species were removed with n-hexane under mild conditions (40 degrees C, 3.4 MPa) and then analytes were extracted with ethyl acetate. The best compromise extraction conditions were 103 degrees C, 13.8 MPa and 3 static extraction cycles of 1 min. The proposed method provided recoveries from 76 to 98%, relative standard deviations under 11% (operating under reproducibility conditions) and quantification limits from 1 to 4 ng/g. The analysis of dust samples from private houses and office buildings confirmed the ubiquitous presence of target bacteriocides in these environments.
Canosa
P
P
Departamento de Química Analítica, Nutrición y Bromatología, Instituto de Investigación y Análisis Alimentario, Universidad de Santiago de Compostela, 15782 Santiago, Spain.
Pérez-Palacios
D
D
Garrido-López
A
A
Tena
M T
MT
Rodríguez
I
I
Rubí
E
E
Cela
R
R
D002853:Chromatography, Liquid / Q000379:methods*; D004391:Dust / Q000032:analysis*; D008401:Gas Chromatography-Mass Spectrometry / Q000379:methods*; D010226:Parabens / Q000032:analysis*; D011312:Pressure; D012680:Sensitivity and Specificity; D014260:Triclosan / Q000032:analysis*
D004391:Dust; D010226:Parabens; D014260:Triclosan