Karthikeyan Sathrugnan, Balasubramanian Rajasekhar, See Siao Wei
Department of Chemical and Biomolecular Engineering, National University of Singapore, Engineering Drive 4, Singapore.
Talanta. 2006 Mar 15;69(1):79-86. doi: 10.1016/j.talanta.2005.08.060. Epub 2005 Nov 10.
A low temperature microwave-assisted extraction method (MAE) is reported for the analysis of polycyclic aromatic hydrocarbons (PAHs) in airborne particulate matter (PM). The main parameters affecting the extraction efficiency (choice of extractants, microwave power, and extraction time) were investigated and optimized. The optimized procedure requires a 20 ml mixture of acetone:n-hexane (1:1) for extraction of PAHs in PM at 150W of microwave energy (20 min extraction time). Clean-up of MAE extracts was not found to be necessary. The optimized method was validated using two different SRM (1648-urban particulate matter and 1649a, urban dust). The results obtained are in good agreement with certified values. PAHs recoveries for both reference materials were between 79 and 122% with relative standard deviation ranging from 3 to 21%. Detection limits were determined based on blank determination using two kinds of quartz filter substrates (n=10), which ranged from 0.001 (0.03) ng m(-3)(pg/microg) for B(k)Ft to 1.119 (37.3) for Naph in ng m(-3) (pg/microg), respectively. The repeatability and day-to-day reproducibility obtained in this study were in the range of 4-16 and 3-25% for spiked standards and SRM 1649, respectively. The optimized and validated MAE technique was applied to the extraction of PAHs from a set of real world PM samples collected in Singapore. The sum of particulate-bound PAHs in outdoor PM ranged from 1.05 to 3.45 ng m(-3) while that in indoor PM (cooking emissions) ranged from 27.6 to 75.7 ng m(-3), respectively.
本文报道了一种低温微波辅助萃取法(MAE)用于分析空气中颗粒物(PM)中的多环芳烃(PAH)。研究并优化了影响萃取效率的主要参数(萃取剂的选择、微波功率和萃取时间)。优化后的方法是使用20 ml丙酮与正己烷(1:1)的混合溶液,在150W微波能量下萃取PM中的PAH(萃取时间20分钟)。结果发现无需对MAE萃取液进行净化处理。使用两种不同的标准参考物质(SRM)(1648 - 城市颗粒物和1649a - 城市灰尘)对优化后的方法进行了验证。所得结果与认证值高度吻合。两种参考物质的PAH回收率在79%至122%之间,相对标准偏差在3%至21%之间。基于使用两种石英滤膜基质(n = 10)的空白测定确定了检测限,B(k)Ft的检测限为0.001(0.03)ng m(-3)(pg/μg),萘的检测限为1.119(37.3)ng m(-3)(pg/μg)。本研究中加标标准物和SRM 1649的重复性和日间重现性分别在4% - 16%和3% - 25%范围内。将优化并验证后的MAE技术应用于从新加坡采集的一组实际PM样品中萃取PAH。室外PM中颗粒结合PAH的总量在1.05至3.45 ng m(-3)之间,而室内PM(烹饪排放)中颗粒结合PAH的总量在27.6至75.7 ng m(-3)之间。