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Sample clean\u2010up is a critical step in the analysis, both in terms of time and cost, indeed. Dispersive liquid\u2013liquid microextraction (DLLME) is a simple and fast extraction based on ternary solvent mixtures that uses small volumes of solvent and sample. A DLLME extraction followed by gas chromatography\u2013mass spectrometry (GC\u2013MS) analysis was developed and validated for the analysis of propofol in blood, urine, and hair. The same extraction mixture of 2.5:1 methanol\/chloroform was used for the different biological samples. Validation for linearity, LOD, LOQ, precision, accuracy, and recovery gave satisfactory results for the three types of biological samples included in the study, with limits of quantification of 1\u2009\u03bcg\/mL for urine, 0.2\u2009\u03bcg\/mL for blood, and 0.1\u2009ng\/mg for hair. The DLLME procedure for purification involves a small amount of solvent, thus reducing the cost and the environmental impact. In addition, a high enrichment factor is obtained, and the time for analysis is short. The method was applied to authentic post\u2010mortem samples for the determination of propofol in blood, urine, and hair. Also, segmental hair analysis was performed to assess chronic propofol abuse. The developed method proved to be rapid, simple, and cost\u2010effective for blood, urine, and hair extract clean\u2010up for the determination of propofol by GC\/MS.<\/jats:p>","DOI":"10.1002\/dta.3856","type":"journal-article","created":{"date-parts":[[2025,1,23]],"date-time":"2025-01-23T00:54:34Z","timestamp":1737593674000},"page":"1528-1536","update-policy":"https:\/\/doi.org\/10.1002\/crossmark_policy","source":"Crossref","is-referenced-by-count":3,"title":["Rapid and Simple Dispersive Liquid\u2013Liquid Microextraction (DLLME) Sample Preparation for Propofol Analysis in Hair, Blood, and Urine by Gas Chromatography\u2013Mass Spectrometry"],"prefix":"10.1002","volume":"17","author":[{"ORCID":"https:\/\/orcid.org\/0000-0002-5143-8649","authenticated-orcid":false,"given":"Sara","family":"Odoardi","sequence":"first","affiliation":[{"name":"Department of Healthcare Surveillance and Bioethics, Forensic Toxicology Laboratory Universit\u00e0 Cattolica del Sacro Cuore, Fondazione Policlinico Universitario A. 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