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Updated: Aug 12, 2026

Integration of Miniaturized Solid Phase Extraction and LC-MS/MS Detection of 3-Nitrotyrosine in Human Urine for Clinical Applications
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Versatile, efficient system for extracting drugs from urine for gas chromatographic/mass spectrometric analysis
1Department of Clinical Biochemistry, University Hospital, London, Ontario, Canada.
Abstract:
This is a method for efficiently extracting a wide variety of drugs from urine for toxicological analysis by gas chromatography/mass spectrometry. Before extraction, the urine sample is acetylated, diluted with an equal volume of water, and saturated with NaCl. This solution is then mixed with an equal volume of dichloromethane/acetone (2:1 by vol). The organic (top) phase is aspirated and evaporated, and the residue is redissolved in a suitable solvent for injection or further derivatization. This procedure is suitable for all drugs except carboxylate-containing drugs, which may be isolated by replacing the acetylation step with acidification of the urine to pH 2. Studies with 16 drugs containing amino, amide, alcoholic hydroxyl, phenolic hydroxyl, carboxylate groups, or combinations thereof, showed that all drugs except theophylline and benzoylecgonine were extracted with analytical recoveries ranging from 70% to 100%.
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