<abstract xmlns="http://www.w3.org/1999/xhtml"><p> A high-throughput liquid chromatography method with detection by tandem mass spectrometry (LC-MS/MS) was developed and validated for the quantification of apixaban in human plasma. The separation was performed on a Gemini-NX column under isocratic conditions using a 33:67 (v/v) mixture of acetonitrile and 1 mM ammonium formate in water at 40 ºC with a flow rate of 0.5 mL/min. The detection of apixaban was performed in multiple reaction monitoring mode (m/z 417.2 from m/z 460.2) with electrospray positive ionization. A single-step protein precipitation with methanol was used for plasma sample preparation. The method was validated with respect to selectivity, linearity (r > 0.994), intra-day and inter-day precision (CV &lt; 14.4 %) and accuracy (bias &lt; 9.5 %) over the range of 9.70 - 970.00 ng/mL plasma. The lower limit of quantification (LLOQ) was 9.70 ng/mL and the recovery was between 97.4 - 104.5 %. The method is fast, efficient, requires the processing of a small volume of plasma (50 μL), a short run-time (1 min) for chromatographic analysis, and a simple and rapid preparation of samples. It is very well suited for clinical therapeutic drug monitoring and pharmacokinetic studies.</p></abstract>

A high-throughput liquid chromatography method with detection by tandem mass spectrometry (LC-MS/MS) was developed and validated for the quantification of apixaban in human plasma. The separation was performed on a Gemini-NX column under isocratic conditions using a 33:67 (v/v) mixture of acetonitrile and 1 mM ammonium formate in water at 40 ºC with a flow rate of 0.5 mL/min. The detection of apixaban was performed in multiple reaction monitoring mode (m/z 417.2 from m/z 460.2) with electrospray positive ionization. A single-step protein precipitation with methanol was used for plasma sample preparation. The method was validated with respect to selectivity, linearity (r > 0.994), intra-day and inter-day precision (CV < 14.4 %) and accuracy (bias < 9.5 %) over the range of 9.70 - 970.00 ng/mL plasma. The lower limit of quantification (LLOQ) was 9.70 ng/mL and the recovery was between 97.4 - 104.5 %. The method is fast, efficient, requires the processing of a small volume of plasma (50 μL), a short run-time (1 min) for chromatographic analysis, and a simple and rapid preparation of samples. It is very well suited for clinical therapeutic drug monitoring and pharmacokinetic studies.

Determination of Apixaban Levels in Human Plasma by a High-Throughput Liquid Chromatographic Tandem Mass Spectrometry Assay / Determinarea rapidă a apixabanului în plasma umană prin cromatografie de lichide de înaltă performanță cuplată cu spectrometrie de masă în tandem

Family Medicine, Department M3 Clinical Sciences Internal Medicine, University of Medicine and Pharmacy, Târgu Mures

Department of Toxicology - Faculty of Pharmacy, “Iuliu Haţieganu” University of Medicine and Pharmacy, Cluj-Napoca

University of Medicine and Pharmacy Tirgu Mures

Department of Clinical Pharmacy - Faculty of Pharmacy, “Iuliu Haţieganu” University of Medicine and Pharmacy, Cluj-Napoca

Department of Anesthesiology and Intensive Care of the University of Medicine and Pharmacy, Targu-Mures

Infectious Diseases, Department M4, University of Medicine and Pharmacy, Târgu Mures

Revista Romana de Medicina de Laborator

This work is licensed under the Creative Commons Attribution-NonCommercial-NoDerivatives 3.0 License.

A high-throughput liquid chromatography method with detection by tandem mass spectrometry (LC-MS/MS) was developed and validated for the quantification of...

Determination of Apixaban Levels in Human Plasma by a High-Throughput Liquid Chromatographic Tandem Mass Spectrometry Assay / Determinarea rapidă a apixabanului în plasma umană prin cromatografie de lichide de înaltă performanță cuplată cu spectrometrie de masă în tandem

Publié en ligne: 25 mars 2015

Pages: 115 - 125

Reçu: 06 déc. 2014

Accepté: 16 févr. 2015

DOI: https://doi.org/10.1515/rrlm-2015-0006

Mots clés
apixaban;LC-MS/MS;therapeutic drug monitoring

© by Daniela Saveta Popa

This work is licensed under the Creative Commons Attribution-NonCommercial-NoDerivatives 3.0 License.

Determination of Apixaban Levels in Human Plasma by a High-Throughput Liquid Chromatographic Tandem Mass Spectrometry Assay / Determinarea rapidă a apixabanului în plasma umană prin cromatografie de lichide de înaltă performanță cuplată cu spectrometrie de masă în tandem

Publié en ligne: 25 mars 2015

Pages: 115 - 125

Reçu: 06 déc. 2014

Accepté: 16 févr. 2015

DOI: https://doi.org/10.1515/rrlm-2015-0006

Mots clésapixaban;LC-MS/MS;therapeutic drug monitoring

© by Daniela Saveta Popa

This work is licensed under the Creative Commons Attribution-NonCommercial-NoDerivatives 3.0 License.

Mots clés
apixaban;LC-MS/MS;therapeutic drug monitoring