Inorganic‐Organic Nanoarchitectonics: MXene/Covalent Organic Framework Heterostructure for Superior Microextraction

Abstract One of the difficulties limiting covalent organic frameworks (COFs) from becoming excellent adsorbents is their stacking/aggregation architectures owing to poor morphology/structure control during the synthesis process. Herein, an inorganic‐organic nanoarchitectonics strategy to synthesize the MXene/COF heterostructure (Ti 3 C 2 T x /TAPT‐TFP) is developed by the assembly of β ‐ketoenamine‐linked COF on the Ti 3 C 2 T x MXene nanosheets. The as‐prepared Ti 3 C 2 T x /TAPT‐TFP retains the 2D architecture and high adsorption capacity of MXenes as well as large specific surface area and hierarchical porous structure of COFs. As a proof of concept, the potential of Ti 3 C 2 T x /TAPT‐TFP for solid‐phase microextraction (SPME) of trace organochlorine pesticides (OCPs) is investigated. The Ti 3 C 2 T x /TAPT‐TFP based SPME method achieves low limits of detection (0.036–0.126 ng g −1 ), wide linearity ranges (0.12–20.0 ng g −1 ), and acceptable repeatabilities for preconcentrating trace OCPs from fruit and vegetable samples. This study offers insights into the potential of constructing COF or MXene‐based heterostructures for the microextraction of environmental pollutants.