Department of Analytical Chemistry, National Institute of Chemistry, Hajdrihova 19, 1000, Ljubljana, Slovenia; Faculty of Chemistry and Chemical Technology, University of Ljubljana, Večna Pot 113, 1000, Ljubljana, Slovenia.
Department of Analytical Chemistry, National Institute of Chemistry, Hajdrihova 19, 1000, Ljubljana, Slovenia.
Talanta. 2023 Jan 1;251:123761. doi: 10.1016/j.talanta.2022.123761. Epub 2022 Jul 31.
In this work, we developed and optimized a method for the analysis of PAHs and nitro-PAHs in atmospheric particulate matter (PM) samples by using thermal desorption gas chromatography coupled with electron ionization single quadrupole mass spectrometry (TD-GC-(EI)-MS). The method uses thermal desorption from a PM on a filter sample as means of sample introduction to a column and obviates the need for complex extraction procedures, which are time-consuming and require environmentally unfriendly solvents. Moreover, the possibility of systematic errors is minimized and a significantly smaller amount of sample is required compared to traditional techniques requiring a pre-extraction step (approx. 10-times). Thirteen PAHs and three nitro-PAHs were used during method development. Although Tenax cartridges are typically used to capture volatile pollutants from the air, we found that glass-wool liner is the most suitable trap for the examined analytes after desorption from a quartz filter. Among the various instrument parameters which were tested and optimized, TD desorption flow and hold time, and temperature of the cooled injection system (CIS) proved to be most critical. We also found out that the matrix effect is especially pronounced in the case of high PM loadings, which should be kept in mind when planning the analysis. After the optimization, standard reference materials (ERM-CZ100 and NIST 1648a) were used for partial method validation and finally, real PM and PM samples from two Slovenian cities were successfully analyzed.
在这项工作中，我们开发并优化了一种通过热解吸气相色谱-电子电离单四极杆质谱（TD-GC-(EI)-MS）分析大气颗粒物（PM）样品中多环芳烃（PAHs）和硝基多环芳烃（NPAHs）的方法。该方法使用从滤膜上的 PM 进行热解吸作为进样手段，而无需复杂的提取程序，这些程序耗时且需要使用对环境不友好的溶剂。此外，与需要预提取步骤的传统技术相比，系统误差的可能性最小，所需的样品量也大大减少（约减少 10 倍）。在方法开发过程中使用了十三种 PAHs 和三种硝基 PAHs。尽管 Tenax 管通常用于捕获空气中的挥发性污染物，但我们发现，经过石英滤膜解吸后，玻璃纤维衬垫是最适合用于分析物的捕集阱。在测试和优化的各种仪器参数中，TD 解吸流量和保持时间以及冷却进样系统（CIS）的温度被证明是最关键的。我们还发现，在高 PM 负载的情况下，基质效应特别明显，在规划分析时应牢记这一点。经过优化后，使用标准参考物质（ERM-CZ100 和 NIST 1648a）进行了部分方法验证，最后成功分析了来自两个斯洛文尼亚城市的实际 PM 和 PM 样品。
