Alvarez-Avilés O, Cuadra-Rodríguez L, González-Illán F, Quiñones-González J, Rosario O
Chemistry Department, University of Puerto Rico, Río Piedras Campus, P.O. Box 23346, San Juan, Puerto Rico.
Anal Chim Acta. 2007 Aug 6;597(2):273-81. doi: 10.1016/j.aca.2007.07.004. Epub 2007 Jul 5.
A practical analytical methodology based on coupling microwave-assisted extraction-stir bar sorptive extraction-thermal desorption-gas chromatography-mass spectrometry (MAE-SBSE-TD-GC-MS) was developed and validated for the characterization of several SVOC in atmospheric particulate matter (PM). The high enrichment capacity of SBSE makes it a powerful tool for improving detection limits and MAE has been useful for overcoming the long extraction times and high volumes of extraction solvent used in traditional methodologies. Relative to Soxhlet extraction followed by GC-MS analysis (EPA Methods 3540 and 8270C), the MAE-SBSE-TD-GC-MS methodology resulted with approximately 10(4) times better detection limits. Detection limits ranged from 0.3 to 8.3 pg m(-3) for pp'-DDD and decachlorobyphenyl, respectively in PM2.5, 24 m3 air sample. The performance of the optimized methodology gave good precisions, with R.S.D. less than 30% for most of the standards, and linearity within the range tested of 0.1-15 microg L(-1). Analysis of real PM samples resulted in the identification of compounds in the ng L(-1) range.
开发并验证了一种基于微波辅助萃取-搅拌棒吸附萃取-热脱附-气相色谱-质谱联用(MAE-SBSE-TD-GC-MS)的实用分析方法,用于表征大气颗粒物(PM)中的几种半挥发性有机化合物(SVOC)。SBSE的高富集能力使其成为提高检测限的有力工具,而MAE有助于克服传统方法中萃取时间长和萃取溶剂量大的问题。相对于索氏萃取后进行GC-MS分析(EPA方法3540和8270C),MAE-SBSE-TD-GC-MS方法的检测限提高了约10⁴倍。在24立方米空气样本的PM2.5中,pp'-滴滴滴和十氯联苯的检测限分别为0.3至8.3 pg m⁻³。优化方法的性能具有良好的精密度,大多数标准品的相对标准偏差(R.S.D.)小于30%,在0.1 - 15 μg L⁻¹的测试范围内具有线性关系。对实际PM样本的分析鉴定出了纳克/升范围内的化合物。