Novel per- and polyfluoroalkyl substances (PFASs) raise global concerns due to their toxic effects on environment and human health. However, researches on analytical methods of novel PFASs are lacking. Here, a kind of selective cationic covalent organic framework (iCOF) was designed and loaded on the surface of cotton as an adsorbent. Then, a simple solid-phase extraction (SPE) method based on the cotton@iCOF was developed for high throughput rapid extraction of six novel PFASs in water samples, coupled with ultrahigh-performance liquid chromatography−tandem mass spectrometry (UHPLC–MS/MS) determination. Several important SPE parameters, such as the amount of iCOF, sample pH, desorption conditions and salinity were systematically investigated. Under optimal conditions, the limits of detection and quantification of this SPE-UHPLC–MS/MS method were as low as 0.08−2.14 ng/L and 0.28−7.15 ng/L, respectively. The recoveries were 77.9−117.6% for the tap water and surface water, and F-53 B in surface water were detected. Notably, this SPE process was rapid (1 h for 500 mL water sample) compared with commercial SPE (normal 2−3 h), owing to little resistance of cotton@iCOF and omission of nitrogen blowing process, and high throughput with 12 samples concurrently extracted. Additionally, various characterization means and density functional theory (DFT) calculations showed that ion-exchange effect, hydrophobic interaction, hydrogen bonding and ordered channel structure synergistically contributed to the PFASs adsorption on cotton@iCOF. The cotton@iCOF-based SPE method with simplicity, rapidity, selectivity and efficiency provided new research ideas for the analysis and control of ionic emerging pollutants in water.

新型全氟烷基物质和多氟烷基物质 (PFAS) 因其对环境和人类健康的毒性影响而引起全球关注。然而，缺乏对新型PFASs分析方法的研究。在这里，一种选择性阳离子共价有机骨架（iCOF）被设计并负载在棉花表面作为吸附剂。然后，开发了一种基于棉花@iCOF 的简单固相萃取 (SPE) 方法，用于高通量快速萃取水样中的六种新型 PFAS，并结合超高效液相色谱-串联质谱 (UHPLC-MS/MS) ） 决心。系统地研究了几个重要的 SPE 参数，例如 iCOF 的量、样品 pH 值、解吸条件和盐度。在最优条件下， 分别为ng/L 和 0.28-7.15  ng/L。自来水和地表水的回收率为77.9-117.6%，地表水中检测到F-53 B。值得注意的是，与商业 SPE（正常 2-3  h），由于cotton@iCOF的阻力小，省略了吹氮过程，同时提取12个样品的通量很高。此外，各种表征手段和密度泛函理论（DFT）计算表明，离子交换效应、疏水相互作用、氢键和有序通道结构协同促进了 PFASs 在棉花@iCOF 上的吸附。基于cotton@iCOF的SPE方法简单、快速、选择性和高效，为水中离子型新兴污染物的分析和控制提供了新的研究思路。