Canosa P, Pérez-Palacios D, Garrido-López A, Tena M T, Rodríguez I, Rubí E, Cela R
Departamento de Química Analítica, Nutrición y Bromatología, Instituto de Investigación y Análisis Alimentario, Universidad de Santiago de Compostela, 15782 Santiago, Spain.
J Chromatogr A. 2007 Aug 17;1161(1-2):105-12. doi: 10.1016/j.chroma.2007.05.089. Epub 2007 Jun 2.
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.
提出了一种基于加压液体萃取的样品制备方法,用于测定室内灰尘中的四种对羟基苯甲酸烷基酯和三氯生。通过在萃取池中放置合适的吸附剂,并选择洗涤和洗脱溶剂的正确组合,在同一步骤中实现了分析物的萃取和干扰物质的去除。化合物以硅烷化衍生物的形式,通过气相色谱结合串联质谱(GC-MS/MS)进行测定。仔细评估了影响样品制备程序产率和选择性的因素。在最终条件下,将干燥的样品(0.5 g灰尘和1 g硫酸钠)与3 g弗罗里硅土分散,装入一个11 mL不锈钢萃取池中,该萃取池中含有1 g作为净化吸附剂的相同材料。在温和条件(40℃,3.4 MPa)下用正己烷去除非极性物质,然后用乙酸乙酯萃取分析物。最佳折衷萃取条件为103℃、13.8 MPa和3次1分钟的静态萃取循环。该方法的回收率为76%至98%,相对标准偏差在11%以下(在重现性条件下操作),定量限为1至4 ng/g。对私人住宅和办公楼灰尘样品的分析证实了这些环境中目标杀菌剂的普遍存在。