An efficient and robust solid-phase microextraction (SPME) fiber was developed for vacuum-assisted sampling of polycyclic aromatic hydrocarbons (PAHs) in solid samples. The surface of a stainless-steel fiber was first oxidized and then coated with nanostructured n-octadecylsilica using the Stober method, by hydrolysis and condensation of tetraethylorthosilicate in the presence of octadecyltrichlorosilane through a sol–gel strategy. The synthesized sorbent was characterized using scanning electron microscopy/energy dispersive X-ray analysis (SEM/EDX) and Fourier transform infrared spectroscopy (FT-IR). The developed vacuum-assisted headspace SPME (VA-HS-SPME) procedure was coupled with GC-FID and optimized for the analysis of PAHs in soil, using multivariate statistical analysis, based on Box-Behnken design. The calibration graphs for seven PAHs were linear (R2 > 0.995) over 0.001-4000 ng g-1. The limits of detection were found to be 0.1-0.9 pg g-1. The relative standard deviations for six repeated analyses of 100 ng g-1 of the PAHs (using a single fiber) were calculated 3.2-8.7% and fiber-to-fiber reproducibility (n = 6) obtained 5.2-12.34%. The nanostructured octadecylsilica was shown to be substantially robust and durable. It was utilized for ultrasensitive VA-HS-SPME/GC analysis of the PAHs in different polluted soil samples and satisfactory results were obtained, with low matrix effects.

中文翻译：

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纳米结构十八烷基二氧化硅化学涂层不锈钢纤维，用于土壤中多环芳烃的真空辅助 HS-SPME 采样

开发了一种高效且坚固的固相微萃取 (SPME) 纤维，用于固体样品中多环芳烃 (PAH) 的真空辅助取样。不锈钢纤维的表面首先被氧化，然后使用 Stober 方法通过溶胶 - 凝胶策略在十八烷基三氯硅烷的存在下水解和缩合原硅酸乙酯的纳米结构正十八烷基二氧化硅涂层。使用扫描电子显微镜/能量色散 X 射线分析 (SEM/EDX) 和傅里叶变换红外光谱 (FT-IR) 对合成的吸附剂进行表征。开发的真空辅助顶空 SPME (VA-HS-SPME) 程序与 GC-FID 相结合，并使用基于 Box-Behnken 设计的多元统计分析对土壤中多环芳烃的分析进行了优化。七种 PAH 的校准图在 0.001-4000 ng g-1 范围内呈线性（R2 > 0.995）。发现检测限为 0.1-0.9 pg g-1。对 100 ng g-1 多环芳烃（使用单根纤维）进行六次重复分析的相对标准偏差计算为 3.2-8.7%，纤维间重现性 (n = 6) 为 5.2-12.34%。纳米结构的十八烷基二氧化硅被证明是非常坚固耐用的。将其用于不同污染土壤样品中多环芳烃的超灵敏 VA-HS-SPME/GC 分析，获得了令人满意的结果，基质效应低。7% 和纤维间再现性 (n = 6) 获得 5.2-12.34%。纳米结构的十八烷基二氧化硅被证明是非常坚固耐用的。将其用于不同污染土壤样品中多环芳烃的超灵敏 VA-HS-SPME/GC 分析，获得了令人满意的结果，基质效应低。7% 和纤维对纤维再现性 (n = 6) 获得 5.2-12.34%。纳米结构的十八烷基二氧化硅被证明是非常坚固耐用的。将其用于不同污染土壤样品中多环芳烃的超灵敏 VA-HS-SPME/GC 分析，获得了满意的结果，基质效应低。