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This study describes the development and validation of an LC\u2013MS\/MS method for the quantification of nitazene analogs and related metabolites in plasma using micro\u2010QuEChERS sample preparation. The validated concentration range was 0.05\u201320\u2009ng\/mL, with coefficients of determination\n                    <jats:italic>R<\/jats:italic>\n                    <jats:sup>2<\/jats:sup>\n                    \u2009&gt;\u20090.99. The limit of detection (LOD) was 0.025\u2009ng\/mL, and the lower limit of quantification (LLOQ) was 0.05\u2009ng\/mL. Bias ranged from \u22122.6% to 15.7%, within\u2010run precision from 3.4% to 12.7%, and between\u2010run precision from 4.4% to 14.9%, as evaluated at three quality control levels. Matrix effects and recovery were analyte\u2010dependent but compatible with satisfactory overall validation performance. No interferences or carryover were observed. Method applicability was demonstrated in an authentic intoxication case, in which\n                    <jats:italic>N<\/jats:italic>\n                    \u2010pyrrolidino protonitazene was quantified at 1.4\u2009ng\/mL, representing, to our knowledge, the first clinical case reported in Brazil. The case was clinically characterized by severe opioid toxicity requiring repeated naloxone administration. The proposed method combined low sample volume, simple sample preparation, and suitable analytical performance for targeted analysis of emerging nitazene compounds. These findings support the use of micro\u2010QuEChERS and LC\u2013MS\/MS as a practical approach for targeted nitazene quantification in clinical and forensic toxicology.\n                  <\/jats:p>","DOI":"10.1002\/dta.70126","type":"journal-article","created":{"date-parts":[[2026,7,29]],"date-time":"2026-07-29T00:10:08Z","timestamp":1785283808000},"page":"1296-1310","update-policy":"https:\/\/doi.org\/10.1002\/crossmark_policy","source":"Crossref","is-referenced-by-count":0,"title":["Micro\u2010QuEChERS Extraction for Broad\u2010Spectrum LC\u2010QQQ\u2010MS Quantification of Nitazene Analogs in Plasma: A Validated Method With Casework Application"],"prefix":"10.1002","volume":"18","author":[{"given":"Karla\u00a0A.\u00a0O.","family":"Souza","sequence":"first","affiliation":[{"name":"Centro de Informa\u00e7\u00e3o e Assist\u00eancia Toxicol\u00f3gica de Campinas (CIATox\u2010Campinas) Universidade Estadual de Campinas (UNICAMP)  Campinas SP Brazil"},{"name":"Faculdade de 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