AbstractThis work presents a comprehensive overview of solidified floating organic drop microextraction, with a particular emphasis on its applications in the analysis of heavy metal ions and different pharmaceutical compounds by sample pretreatment, complexation, and their identification by various analytical techniques. Here, we discussed basic principles, procedures, applications of the technique, and effects of different variables like pH, temperature, stirring rate, extraction time, salts addition, extraction solvent and extraction volume, centrifugation speed, and, vortex time on preconcentration. In brief, the review summarises the various modes of solidified floating organic drop microextraction such as dispersive liquid‐liquid microextraction, ultrasound‐assisted, air‐assisted liquid‐liquid microextraction, and vortex‐assisted solidified floating organic drop microextraction. this review covers the methods combined with analytical techniques such as inductively coupled plasma‐optical emission spectrometry, electrothermal atomic absorption spectrometry, flame atomic absorption spectroscopy, graphite furnace atomic absorption spectrometry, electrothermal vaporization inductively coupled plasma mass spectrometry, high‐performance liquid chromatography, and gas chromatography/mass spectrometry. among these, the incorporation of ultrasonic, vortex, and air agitation improves the dispersion mechanism. The coupling of solidified floating organic drop microextraction with other techniques enhances the selectivity and efficiency of the preconcentration procedure. This review provides a potential overview of the fundamental principles, advancements in various modes, influencing factors, and applications of solidified floating organic drop microextraction, showing its potential for advancements in sample preparation and analytical methodologies across various domains.