Department of Chemistry & Biochemistry, The University of Texas at Arlington, 700 Planetarium Place, Arlington, TX 76019, USA.
Shimadzu Corporation, 1,Nishinokyo Kuwabara-cho, Nakagyo-ku, Kyoto 604-8511, Japan.
J Chromatogr B Analyt Technol Biomed Life Sci. 2018 Jun 1;1086:82-88. doi: 10.1016/j.jchromb.2018.04.014. Epub 2018 Apr 11.
On-line supercritical fluid extraction - supercritical fluid chromatography - mass spectrometry (SFE-SFC-MS) has been applied for the determination of polycyclic aromatic hydrocarbons (PAHs) in soil. The purpose of this study was to develop and validate the first on-line SFE-SFC-MS method for the quantification of PAHs in various types of soil. By coupling the sample extraction on-line with chromatography and detection, sample preparation is minimized, diminishing sample loss and contamination, and significantly decreasing the required extraction time. Parameters for on-line extraction coupled to chromatographic analysis were optimized. The method was validated for concentrations of 10-1500 ng of PAHs per gram of soil in Certified Reference Material (CRM) sediment, clay, and sand with R ≥ 0.99. Limits of detection (LOD) were found in the range of 0.001-5 ng/g, and limits of quantification (LOQ) in the range of 5-15 ng/g. The method developed in this study can be effectively applied to the study of PAHs in the environment, and may lay the foundation for further applications of on-line SFE-SFC-MS.
在线超临界流体萃取-超临界流体色谱-质谱联用(SFE-SFC-MS)已被应用于土壤中多环芳烃(PAHs)的测定。本研究旨在开发和验证首个在线 SFE-SFC-MS 方法,用于定量分析各种类型土壤中的 PAHs。通过将样品在线萃取与色谱和检测相耦合,最小化了样品制备,减少了样品损失和污染,并显著缩短了所需的提取时间。对在线萃取与色谱分析相结合的参数进行了优化。该方法在认证参考物质(CRM)沉积物、粘土和沙子中 PAHs 浓度为 10-1500ng/g 时进行了验证,相关系数(R)≥0.99。检测限(LOD)在 0.001-5ng/g 范围内,定量限(LOQ)在 5-15ng/g 范围内。本研究中开发的方法可有效应用于环境中 PAHs 的研究,并可能为进一步应用在线 SFE-SFC-MS 奠定基础。