Porous materials have great prospective applications for solid-phase microextraction (SPME) technology because of their large specific surface area and pore volume. In this study, a hierarchical porous carbon (HPC) was synthesized by simple hydrothermal reaction and potassium hydroxide (KOH) activation of crude biomass and found to be an efficient adsorbent for SPME of organic pollutants. Results show that the as-prepared HPC has a partly graphitic amorphous-like structure with ultrahigh specific surface area (2551 m²/g), high pore volume (1.53 cm³/g), good pore size distribution (PSD) (mesopore/micropore ratio of 68%), and great thermal stability (>450 °C). When we utilized it as SPME fiber coating, the extraction capacities for chlorobenzenes (CBs), polychlorinated biphenyls (PCBs), polycyclic aromatic hydrocarbons (PAHs), and phthalates (PAEs) were, respectively, 1.13–39.46, 2.40–7.78, 1.34–36.02, and 1.50–1.83 times higher than those of a commercial polydimethylsiloxane (PDMS) fiber. Under the optimized extraction conditions, an analytical method for CBs with low detection limits (0.01–0.24 ng/L), good repeatability (1.00%–4.93% for intra-day, 1.11%–6.94% for inter-day), and great reproducibility (1.48%–8.91%, n = 3) was developed. Moreover, we evaluated the practicality of the developed method for environmental water sample and obtained satisfactory recoveries (86.21%–104.34%). The findings provide a novel and promising HPC from crude biomass using a low-cost and facile synthetic route for SPME applications.

多孔材料因其大的比表面积和孔体积而在固相微萃取（SPME）技术中具有广阔的应用前景。在这项研究中，通过简单的水热反应和粗生物质的氢氧化钾（KOH）活化合成了分层多孔碳（HPC），发现它是有机污染物SPME的有效吸附剂。结果表明，所制备的HPC具有部分石墨无定形的结构，具有超高的比表面积（2551 m ² / g），高孔体积（1.53 cm ^3）/ g），良好的孔径分布（PSD）（中孔/微孔比率为68％）和良好的热稳定性（> 450°C）。当我们将其用作SPME纤维涂层时，氯苯（CBs），多氯联苯（PCBs），多环芳烃（PAHs）和邻苯二甲酸酯（PAEs）的萃取容量分别为1.13–39.46、2.40–7.78、1.34–比市售的聚二甲基硅氧烷（PDMS）纤维高36.02倍和1.50–1.83倍。在优化的萃取条件下，对CB的分析方法检出限低（0.01–0.24 ng / L），重复性好（日内为1.00％–4.93％，日间为1.11％–6.94％），并且具有很好的重现性开发了可重复性（1.48％–8.91％，n = 3）。此外，我们评估了开发的环境水样方法的实用性，并获得了令人满意的回收率（86.21％–104.34％）。