Yusà V, Quintas G, Pardo O, Pastor A, Guardia M de la
Public Health Laboratory of Valencia, Generalitat Valenciana, C/Micer Mascó 31, 46010-Valencia, Spain.
Talanta. 2006 Jun 15;69(4):807-15. doi: 10.1016/j.talanta.2005.11.018. Epub 2005 Dec 15.
A sensitive and automated method is presented for the determination of polycyclic aromatic hydrocarbons (PAHs) in airborne particulate matter. The procedure includes extraction of PM10-bound PAHs by accelerated solvent extraction (ASE) followed by gel permeation chromatography (GPC) clean-up, and large-volume programmable temperature vaporizer (PTV-LV) injection coupled to GC-MS. The limit of detection (LOD) of the whole method, based on a signal-to-noise ratio (S/N) of 3:1, ranged from 0.26pgm(-3) to 3pgm(-3) when air volumes of 760m(3) are collected. The hexane-acetone mixture (1:1, v/v) gave the best recoveries when ASE parameters were fixed at 125 degrees C, 1500psi, and a total time of 10min. The recoveries for all PAHs tested ranged from 96% to 103%, rates similar to those obtained by the Soxhlet reference method. To improve the sensitivity, 70muL were injected. The PTV-LV injection settings were optimized using a statistical design of experiments, including a screening 2(4) full factorial design and a further central composite design. A sensitivity increase from 10 to 50 times was achieved as compared with the conventional 2muL splitless injection. The method was validated with the standard reference material SRM 1649a and applied to real PM10 samples from the monitoring network of the Regional Valencia Government (Spain). The analytical performance of the method shows that it is appropriate to monitor PAHs levels in ambient air according to European Union Directives. In addition, the method can be used when a high sensitivity is required.
本文介绍了一种灵敏且自动化的方法，用于测定空气中颗粒物中的多环芳烃（PAHs）。该方法包括通过加速溶剂萃取（ASE）提取与PM10结合的PAHs，随后进行凝胶渗透色谱（GPC）净化，以及采用大体积可编程温度汽化器（PTV-LV）进样并与气相色谱-质谱联用（GC-MS）。当采集760立方米空气体积时，基于3:1的信噪比（S/N），整个方法的检测限（LOD）范围为0.26皮克/立方米至3皮克/立方米。当ASE参数固定为125℃、1500磅力/平方英寸和总时间10分钟时，己烷-丙酮混合物（1:1，v/v）的回收率最佳。所有测试PAHs的回收率范围为96%至103%，与索氏提取参考方法获得的回收率相似。为提高灵敏度，进样70微升。采用实验的统计设计对PTV-LV进样设置进行了优化，包括筛选2⁴全因子设计和进一步的中心复合设计。与传统的2微升不分流进样相比，灵敏度提高了10至50倍。该方法用标准参考物质SRM 1649a进行了验证，并应用于西班牙巴伦西亚自治区政府监测网络的实际PM10样品。该方法的分析性能表明，根据欧盟指令，它适用于监测环境空气中的PAHs水平。此外，当需要高灵敏度时也可使用该方法。
