Regueiro Jorge, Llompart Maria, García-Jares Carmen, Cela Rafael
Departamento de Química Analítica, Nutrición y Bromatología, Instituto de Investigación y Análisis Alimentario, Universidad de Santiago de Compostela, Santiago de Compostela 15782, Spain.
J Chromatogr A. 2006 Dec 22;1137(1):1-7. doi: 10.1016/j.chroma.2006.09.080. Epub 2006 Oct 12.
In this paper, a rapid and simple method for the analysis of polybrominated diphenyl ethers (PBDEs) in house dust samples based on microwave-assisted solvent extraction (MASE) and gas chromatography-tandem mass spectrometry (GC-MS/MS) is presented. Extraction conditions were optimized using a multifactorial experimental design approach. The use of an aqueous NaOH phase in combination with a non-polar organic phase (hexane) to extract the target analytes from dust allowed an efficient extraction and reduced chromatographic background. The final hexane extracts could be analyzed after a simple one-step cleanup procedure using Florisil. The validation of the method was performed in terms of accuracy, linearity, and repeatability. The limits of detection (LODs) ranged from 0.29 to 0.55 ng/g for all compounds. The target PBDEs were found in several real dust samples collected in urban and rural houses of Northwestern Spain.
本文介绍了一种基于微波辅助溶剂萃取（MASE）和气相色谱 - 串联质谱（GC-MS/MS）的快速简便的室内灰尘样品中多溴二苯醚（PBDEs）分析方法。采用多因素实验设计方法优化了萃取条件。使用NaOH水相和非极性有机相（己烷）从灰尘中萃取目标分析物，实现了高效萃取并降低了色谱背景。最终的己烷萃取物经过使用弗罗里硅土的简单一步净化程序后即可进行分析。该方法在准确性、线性和重复性方面进行了验证。所有化合物的检测限（LOD）范围为0.29至0.55 ng/g。在西班牙西北部城乡房屋采集的多个实际灰尘样品中发现了目标PBDEs。
