Covalent organic nanospheres (CONs) were explored as a fiber coating for solid-phase microextraction of genotoxic impurities (GTIs) from active ingredients (AIs). CONs were synthesized by an easy solution-phase procedure at 25 °C. The obtained nanospheres exhibited a high specific surface area, good thermostability, high acid and alkali resistance, and favorable crystallinity and porosity. Two types of GTIs, alkyl halides (1-iodooctane, 1-chlorobenzene, 1-bromododecane, 1,2-dichlorobenzene, 1-bromooctane, 1-chlorohexane, and 1,8-dibromooctane) and sulfonate esters (methyl p-toluenesulfonate and ethyl p-toluenesulfonate), were chosen as target molecules for assessing the performance of the coating. The prepared coating achieved high enhancement factors (5097–9799) for the selected GTIs. The strong affinity between CONs and GTIs was tentatively attributed to π–π and hydrophobicity interactions, large surface area of the CONs, and size-matching of the materials. Combined with gas chromatography-mass spectrometry (GC-MS), the established analytical method detected the GTIs in capecitabine and imatinib mesylate samples over a wide linear range (0.2–200 ng/g) with a low detection limit (0.04–2.0 ng/g), satisfactory recovery (80.03%–109.5%), and high repeatability (6.20%–14.8%) and reproducibility (6.20%–14.1%). Therefore, the CON-coated fibers are promising alternatives for the sensitive detection of GTIs in AI samples.

共价有机纳米球（CONs）被探索作为一种纤维涂层，用于从活性成分（AIs）中固相微萃取基因毒性杂质（GTIs）。CONs 是在 25 °C 下通过简单的溶液相程序合成的。所得纳米球具有较高的比表面积、良好的热稳定性、较高的耐酸碱性能以及良好的结晶度和孔隙率。两种类型的 GTI，卤代烷（1-碘辛烷、1-氯苯、1-溴十二烷、1,2-二氯苯、1-溴辛烷、1-氯己烷和 1,8-二溴辛烷）和磺酸酯（对甲苯磺酸甲酯和乙基磷-甲苯磺酸盐）被选为评估涂层性能的目标分子。对于选定的 GTI，制备的涂层实现了高增强因子 (5097-9799)。CONs 和 GTI 之间的强亲和力初步归因于 π-π 和疏水性相互作用、CONs 的大表面积和材料的尺寸匹配。结合气相色谱-质谱（GC-MS），建立的分析方法检测卡培他滨和甲磺酸伊马替尼样品中的 GTI 在宽线性范围（0.2-200 ng/g）内检测限低（0.04-2.0 ng/g）。 g)、良好的回收率（80.03%~109.5%）、高重复性（6.20%~14.8%）和重现性（6.20%~14.1%）。因此，CON 涂层纤维是用于灵敏检测 AI 样品中 GTI 的有希望的替代品。