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Paula Melo

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Papers by Paula Melo

Research paper thumbnail of Benzodiazepine Stability in Postmortem Samples Stored at Different Temperatures

Journal of Analytical Toxicology, 2012

Research paper thumbnail of Analysis of digoxin and metildigoxin in whole blood using solid-phase extraction and liquid chromatography tandem mass spectrometry

International journal of analytical chemistry, 2012

A simple and rapid UPLC/MS/MS method has been developed and validated for the analysis of digoxin... more A simple and rapid UPLC/MS/MS method has been developed and validated for the analysis of digoxin and metildigoxin in whole blood. Samples were prepared by SPE extraction with Oasis HLB columns. Separation was achieved with an ACQUITY UPLC HSS T3 column (2.1 × 100; 1.8 μm), at 35°C. The mobile phase consisted of acetonitrile (70%) and ammonium formate 5 mM (30%). Total run time was 1.5 min operating at isocratic mode with a flow rate of 0.3 mL/min. Mass spectrometry detection was performed by positive mode electrospray, on the ammonium adducts with two transitions for each analyte and one for the IS (d(3)-digoxin). The method proved to be specific and linear over the range (0.3-10) ng/mL. This technique also showed high sensitivity with a 0.09 ng/mL LOD and a 0.28 ng/mL LOQ, for both substances. Percentage recovery ranged from 83 to 100% for digoxin and from 62 to 94% for metildigoxin. The intra- and interday precision CV were ≤10%.

Research paper thumbnail of Benzodiazepine Stability in Postmortem Samples Stored at Different Temperatures

Journal of Analytical Toxicology, 2012

Research paper thumbnail of Analysis of digoxin and metildigoxin in whole blood using solid-phase extraction and liquid chromatography tandem mass spectrometry

International journal of analytical chemistry, 2012

A simple and rapid UPLC/MS/MS method has been developed and validated for the analysis of digoxin... more A simple and rapid UPLC/MS/MS method has been developed and validated for the analysis of digoxin and metildigoxin in whole blood. Samples were prepared by SPE extraction with Oasis HLB columns. Separation was achieved with an ACQUITY UPLC HSS T3 column (2.1 × 100; 1.8 μm), at 35°C. The mobile phase consisted of acetonitrile (70%) and ammonium formate 5 mM (30%). Total run time was 1.5 min operating at isocratic mode with a flow rate of 0.3 mL/min. Mass spectrometry detection was performed by positive mode electrospray, on the ammonium adducts with two transitions for each analyte and one for the IS (d(3)-digoxin). The method proved to be specific and linear over the range (0.3-10) ng/mL. This technique also showed high sensitivity with a 0.09 ng/mL LOD and a 0.28 ng/mL LOQ, for both substances. Percentage recovery ranged from 83 to 100% for digoxin and from 62 to 94% for metildigoxin. The intra- and interday precision CV were ≤10%.

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