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The analytes were completely extracted from the matrix after a short alkaline incubation, and the extracts were further cleaned up by solid\u2010phase extraction using mixed\u2010mode cartridges. Linearity was obtained from 0.1 (lower limit of quantitation, LLOQ) to 30\u2009ng\/mg for both compounds, with correlation coefficients higher than 0.99. Intra\u2010 and interday precision and accuracy were in conformity with internationally accepted guidelines for bioanalytical method validation, and the cleanup procedure presented mean extraction efficiencies higher than 90% for both analytes. This high efficiency greatly contributed to the low limits of quantitation achieved, and therefore this method can be successfully applied in the determination of methadone and EDDP in hair samples in clinical and forensic scenarios where these compounds are involved. 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