Sample preparation maintains a key bottleneck in the whole analytical procedure. Solid‐phase sorbents (SPSs) have garnered increasing attention in sample preparation research due to their crucial roles in achieving high clean‐up and enrichment efficiency in the analysis of trace targets present in complex matrices. Novel nanoscale materials with improved characteristics have garnered considerable interest across different scientific disciplines due to the limited capabilities of traditional bulk‐scale materials. The purpose of this review is to offer a thorough summary of the latest developments and uses of SPSs in preparing samples for chromatographic analysis, focusing on the years 2020–2024. The techniques for preparing SPSs are examined, such as metal–organic frameworks (MOFs), covalent organic frameworks (COFs), carbon nanoparticles (CNPs), molecularly imprinted polymers (MIPs), and metallic nanomaterials (MNs). Examining the pros and cons of different extraction methods, including solid‐phase extraction (SPE), magnetic SPE (MSPE), flow‐based SPE (FBA‐SPE), solid‐phase microextraction (SPME), stir‐bar sorptive extraction (SBSE), and dispersive SPE (DSPE), is the main focus. Furthermore, this article presents the utilization of SPE technology for isolating common contaminants in various environmental, biological, and food specimens. We highlight the persistent challenges in SPSs and anticipate future advancements and applications of novel SPSs.