Department of Chemistry, Faculty of Science, Lorestan University, Khoramabad, Iran.
Department of Chemistry, Faculty of Science, Lorestan University, Khoramabad, Iran.
Anal Chim Acta. 2020 Aug 15;1125:128-134. doi: 10.1016/j.aca.2020.05.067. Epub 2020 May 29.
A headspace microextraction by packed sorbent technique (HS-MEPS) was developed that is assisted by cooling the extraction phase and, in the same time, heating the sample matrix. The innovated cooling assisted HS-MEPS system was optimized for the extraction and HPLC determination of volatile polycyclic aromatic hydrocarbons (PAHs) in solid samples. Amino ethyl-functionalized SBA-15 was used as a nanoporous sorbent for packing the conical hub of the MEPS syringe. For efficient extraction of PAHs, several parameters such as the nature and mass of sorbent, eluent type, elution volume, extraction temperature and number of draw-eject cycles of the syringe were studied and optimized. Under the optimal experimental conditions, only 2 mg of the sorbent was sufficient by applying a temperature of 0 °C to the sorbent while the sample was heated up to 150 °C. Linear calibration curves (R > 0.95) were obtained for all the studied PAHs and their quantitation limits were in the range of 0.042-0.25 ng g. The method was successfully applied to the extraction and HPLC analysis of PAHs in some polluted soil samples.
开发了一种顶空微萃取（HS-MEPS）技术，通过冷却萃取相和同时加热样品基质来辅助。创新的冷却辅助 HS-MEPS 系统经过优化，可用于萃取和高效液相色谱法（HPLC）测定固体样品中的挥发性多环芳烃（PAHs）。氨基乙基功能化的 SBA-15 被用作 MEPS 注射器锥形轮毂的纳米多孔吸附剂。为了有效萃取 PAHs，研究并优化了几个参数，例如吸附剂的性质和质量、洗脱液类型、洗脱体积、萃取温度和注射器的抽提-注射循环次数。在最佳实验条件下，仅需 2 mg 的吸附剂，同时将吸附剂的温度降至 0°C，而将样品加热至 150°C。所有研究的 PAHs 均获得了线性校准曲线（R>0.95），其定量限在 0.042-0.25 ng g 范围内。该方法成功应用于一些污染土壤样品中 PAHs 的萃取和 HPLC 分析。
