This research introduces a novel solid-phase microextraction technology, in which the features of heating of sample, cooling of sorbent, and extraction under vacuum condition have been merged. Heating-, cooling- and vacuum-assisted solid-phase microextraction (HCV-SPME) method was developed as an efficient solution for the direct extraction of volatile and semi-volatiles species in complex solid samples. HCV-SPME was coupled with an in-needle capillary adsorption trap (HCV-INCAT) and applied to the direct extraction of polycyclic aromatic hydrocarbons (PAHs) within soil samples. It consisted of polythiophene/carboxylic acid modified multi-walled carbon nanotube nanocomposite, which was synthesized and wall-coated within a platinized stainless-steel needle via electropolymerization. The influential experimental variables (desorption conditions, sample temperature, adsorption temperature, sampling flow rate, and vacuum level) on the extraction efficiency were optimized. The developed HCV-INCAT technique was used in conjunction with GC-FID and applied for the extraction and determination of PAHs in contaminated soil samples, closely matching with those obtained using a validated ultrasonic-assisted solvent extraction procedure. Under the optimal conditions, linear dynamic ranges, limits of detection, and relative standard deviations were obtained 0.007–5 µg g −1 , 8–20 pg g −1 , and 7.1–12.1%, respectively, for direct extraction of naphthalene, fluorene, phenanthrene, fluoranthene, and pyrene from solid samples.

中文翻译：

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加热、冷却和真空辅助固相微萃取 (HCV-SPME) 用于对复杂基质中的环境污染物进行有效采样

本研究引入了一种新的固相微萃取技术，该技术融合了样品加热、吸附剂冷却和真空条件下萃取的特点。加热、冷却和真空辅助固相微萃取 (HCV-SPME) 方法被开发为直接萃取复杂固体样品中挥发性和半挥发性物质的有效解决方案。HCV-SPME 与针内毛细管吸附阱 (HCV-INCAT) 相结合，应用于直接提取土壤样品中的多环芳烃 (PAH)。它由聚噻吩/羧酸改性的多壁碳纳米管纳米复合材料组成，通过电聚合在镀铂的不锈钢针内合成并壁涂覆。有影响的实验变量（解吸条件、样品温度、吸附温度、取样流速和真空度）对萃取效率的影响。开发的 HCV-INCAT 技术与 GC-FID 结合使用，用于提取和测定受污染土壤样品中的多环芳烃，与使用经过验证的超声波辅助溶剂提取程序获得的那些紧密匹配。在最佳条件下，直接提取萘、芴的线性动态范围、检测限和相对标准偏差分别为 0.007–5 µg g -1 、8–20 pg g -1 和 7.1–12.1% 、菲、荧蒽和芘从固体样品中分离出来。开发的 HCV-INCAT 技术与 GC-FID 结合使用，用于提取和测定受污染土壤样品中的多环芳烃，与使用经过验证的超声波辅助溶剂提取程序获得的样品密切匹配。在最佳条件下，直接提取萘、芴的线性动态范围、检测限和相对标准偏差分别为 0.007–5 µg g -1 、8–20 pg g -1 和 7.1–12.1% 、菲、荧蒽和芘从固体样品中分离出来。开发的 HCV-INCAT 技术与 GC-FID 结合使用，用于提取和测定受污染土壤样品中的多环芳烃，与使用经过验证的超声波辅助溶剂提取程序获得的那些紧密匹配。在最佳条件下，直接提取萘、芴的线性动态范围、检测限和相对标准偏差分别为 0.007–5 µg g -1 、8–20 pg g -1 和 7.1–12.1% 、菲、荧蒽和芘从固体样品中分离出来。