Ratola Nuno, Lacorte Sílvia, Alves Arminda, Barceló Damià
LEPAE, Departamento de Engenharia Química, Faculdade de Engenharia da Universidade do Porto, Rua Dr. Roberto Frias, 4200-465 Porto, Portugal.
J Chromatogr A. 2006 May 12;1114(2):198-204. doi: 10.1016/j.chroma.2006.03.110. Epub 2006 Apr 18.
Three extraction methodologies (Soxhlet, ultrasonic and pressurized liquid extraction) and several clean-up procedures (Florisil, silica and alumina in cartridges or glass column format) were tested and compared to extract 16 US Environmental Protection Agency (EPA) polycyclic aromatic hydrocarbons (PAHs) from Pinus pinea L. needles. Quantification was done by gas chromatography with mass spectrometry, by internal standard method using five deuterated PAH surrogate standards. Among the several extraction and clean-up procedures tested, ultrasonic extraction followed by alumina cartridge clean-up was the preferred method, yielding recoveries between 72 and 100% and limits of detection between 0.22 and 0.71 ng/g dry weight. The performance of the method was tested to determine PAHs in naturally contaminated samples.
测试并比较了三种提取方法(索氏提取法、超声提取法和加压液体提取法)以及几种净化程序(柱式或玻璃柱形式的弗罗里硅土、硅胶和氧化铝),用于从意大利石松针叶中提取16种美国环境保护局(EPA)多环芳烃(PAHs)。采用气相色谱 - 质谱联用仪,通过使用五种氘代多环芳烃替代标准品的内标法进行定量分析。在所测试的几种提取和净化程序中,超声提取法随后用氧化铝柱净化是首选方法,回收率在72%至100%之间,检测限在0.22至0.71 ng/g干重之间。测试了该方法在测定天然污染样品中多环芳烃的性能。