A headspace-hollow fiber solid-phase microextraction (HS-HFSPME) as a selective and sensitive procedure was developed to extract benzene, toluene, ethylbenzene, and p-xylene (BTEX) prior to their determination with gas chromatography-flame ionization detection. δ-Al₂O₃@SiO₂@CTAB core–shell was synthesized as a novel sorbent for the BTEX extraction and enforced into the surface pores on the polypropylene hollow fiber (HF) using sol–gel procedure. The preparation of an HF device for HS-HFSPME can be highly regarded for creating a cheap disposable tool with no memory effects. A chemometric approach, including the Plackett–Burman design and the central composite design, was utilized to optimize the effective factors due to a low number of experiments and investigate the factor interaction. The method shows low LODs (≤ 0.01 ng ml⁻¹), wide linearity, high preconcentration factor (≥ 265), and suitable RSDs (≤ 5.2%) toward the BTEX determination. The method was finally applied to measure BTEX in Buxus leaves and wastewater samples with high recoveries in the range of 89.7–103.4 and low RSD% in the range of 4.64–6.20%, showing the method has suitable recoveries and repeatability. The results confirm that the HS-HFSPME-GC/FID method is an excellent procedure to measure BTEX in various real samples such as plant and wastewater samples with great benefits such as low organic solvent consumption, simple operation, and high sensitivity for the BTEX determination.

开发了顶空-中空纤维固相微萃取 (HS-HFSPME) 作为一种选择性和灵敏的程序来提取苯、甲苯、乙苯和对二甲苯 (BTEX)，然后再用气相色谱-火焰电离检测进行测定。δ-Al ₂ O ₃ @SiO ₂@CTAB 核壳被合成为一种用于 BTEX 提取的新型吸附剂，并使用溶胶-凝胶程序强制进入聚丙烯中空纤维 (HF) 的表面孔中。为 HS-HFSPME 准备 HF 设备可以高度重视创建廉价的一次性工具，没有记忆效应。由于实验次数少，使用化学计量学方法，包括 Plackett-Burman 设计和中心复合设计，来优化有效因子并研究因子相互作用。该方法显示低 LOD（≤ 0.01 ng ml ^-1)、宽线性、高预浓缩因子 (≥ 265) 和适合 BTEX 测定的 RSD (≤ 5.2%)。该方法最终用于测定黄杨树叶和废水样品中的 BTEX，回收率高，范围为 89.7-103.4，RSD% 低，范围为 4.64-6.20%，表明该方法具有合适的回收率和重复性。结果证实 HS-HFSPME-GC/FID 方法是测量各种实际样品（如工厂和废水样品）中 BTEX 的绝佳方法，具有有机溶剂消耗低、操作简单和 BTEX 测定灵敏度高等优点.