Sensitive, accurate, and simultaneous determination of nitrobenzene compounds (NBs) in environmental water samples is of great significance due to their high risk to human health. In this work, a new triazine-based hyper-crosslinked polymer named CC-Py was constructed via the Friedel-Crafts reaction between cyanuric chloride (CC), pyridine (Py) and 1,2-dichloroethane. Due to its excellent stability, high surface area and hydrophilic-lipophilic (amphiphilic) structure, the CC-Py exhibited a high affinity toward the NBs (nitrobenzene, 2-nitrotoluene, 2,6-dimethylnitrobenzene, 3-nitrotoluene, 4-nitrotoluene, 3-nitrochlorobenzene, 4-nitrochlorobenzene, 2-nitrochlorobenzene, 2,4-dimethylnitrobenzene, 3-nitrobromobenzene, 4-nitrobromobenzene and 4-nitroiodobenzene). Then, a CC-Py based solid-phase microextraction coupled with gas chromatography-flame ionization detection was developed to detect the twelve NBs in real water samples. The results showed that the method had low limits of detection (0.20–0.50 μg L⁻¹), good reproducibility (relative standard deviations (RSDs) < 8.6%) and high enrichment factors (967–1590). The recoveries for the NBs in six different types of water samples were between 90% and 111% with the RSDs less than 7.5%. This work provides a facile and sensitive method for the determination of trace level of NBs in real water samples.

环境水样中硝基苯化合物 (NBs) 的灵敏、准确和同时测定具有重要意义，因为它们对人类健康具有高风险。在这项工作中，通过氰尿酰氯 (CC)、吡啶 (Py) 和 1,2-二氯乙烷之间的 Friedel-Crafts 反应构建了一种名为 CC-Py 的新型三嗪基超交联聚合物。由于其出色的稳定性、高表面积和亲水亲油（两亲）结构，CC-Py 对 NBs（硝基苯、2-硝基甲苯、2,6-二甲基硝基苯、3-硝基甲苯、4-硝基甲苯、 3-硝基氯苯、4-硝基氯苯、2-硝基氯苯、2,4-二甲基硝基苯、3-硝基溴苯、4-硝基溴苯和4-硝基碘苯）。然后，开发了基于 CC-Py 的固相微萃取与气相色谱-火焰离子化检测相结合的方法来检测实际水样中的 12 种 NB。结果表明，该方法具有较低的检测限（0.20–0.50 μg·L⁻¹ )、良好的重现性（相对标准偏差 (RSD) < 8.6%）和高富集因子 (967–1590)。六种不同类型水样中 NB 的回收率在 90% 和 111% 之间，RSD 小于 7.5%。本工作为实际水样中痕量 NBs 的测定提供了一种简便、灵敏的方法。