<p>Sample preparation is a crucial phase in the analytical procedure. Recently, nanoparticles and lab-in-syringe (LIS) solid-phase microextraction (SPME) have garnered significant interest from researchers aiming to develop microextraction techniques for sample preparation. Lab-in-syringe (LIS) represents a novel methodology in analytical chemistry that consolidates sample handling, extraction, and occasionally detection into a singular syringe-based apparatus. The LIS approach, when integrated with SPME, presents numerous critical advantages, enhancing its relevance in sample preparation and analysis. The closed environment of the syringe facilitates enhanced regulation of extraction parameters (e.g., mixing, temperature, and timing), hence augmenting the efficiency and sensitivity of SPME. This review elucidates the function of syringes in SPME methods, emphasizing the utilization of nanoparticles as effective sorbents owing to their significantly elevated surface area to volume ratio relative to traditional materials, which provides increased binding sites and enhances extraction efficiency and analyte capacity. A complete description of the many forms of SPME, sorbents, syringes, the functions of syringes, multiple techniques of LIS, and types of nanoparticles that provide variable extraction mechanisms for lab-in-syringe solid-phase microextraction (LIS-SPME). LIS-SPME presents a promising avenue for novel research and assists in the selection of effective and economically viable methodologies, contingent upon the analyte. The benefits of LIS-SPME render it especially simplicity without the necessity for specialized equipment, affordability, less solvent usage and waste production.</p>