Quantification of mycophenolic acid in human plasma by liquid chromatography with time-of-flight mass spectrometry for therapeutic drug monitoring
| Autor: | Nina Ince, Karin Kipper, Jason Raymond, Natalicia J. Antunes, Lewis Couchman, Atholl Johnston, Gilberto De Nucci, David W. Holt |
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| Rok vydání: | 2020 |
| Předmět: |
Electrospray
Analyte Spectrometry Mass Electrospray Ionization Formic acid Clinical Biochemistry 030226 pharmacology & pharmacy 01 natural sciences Biochemistry Sensitivity and Specificity Analytical Chemistry 03 medical and health sciences chemistry.chemical_compound 0302 clinical medicine Drug Discovery External quality assessment medicine Protein precipitation Humans Molecular Biology Pharmacology Reproducibility Chromatography medicine.diagnostic_test Chemistry 010401 analytical chemistry Reproducibility of Results General Medicine Mycophenolic Acid 0104 chemical sciences Therapeutic drug monitoring Linear Models Time-of-flight mass spectrometry Drug Monitoring Immunosuppressive Agents Chromatography Liquid |
| Zdroj: | Biomedical chromatography : BMCREFERENCES. 35(3) |
| ISSN: | 1099-0801 |
| Popis: | This study presents, for the first time, the development and validation of a liquid chromatography and time-of-flight mass-spectrometry (LC-TOF-MS) based assay to quantify mycophenolic acid (MPA) in patient samples as part of a routine therapeutic drug monitoring service. MPA was extracted from 50 μl human plasma by protein precipitation, using sulindac as internal standard (IS). Separation was obtained on a Luna™ Omega polar C18 column kept at 40°C. The mobile phase consisted of a mixture of acetonitrile-deionized water (50:50, v/v) with 0.1% formic acid at a flow rate of 350 μl/min. Analyte and IS were monitored on a TOF-MS using a Jet-Stream™ (electrospray) interface running in positive mode. Assay performance was evaluated by analysing patient plasma (N = 69) and external quality assessment (N = 6) samples. The retention times were 2.66 and 2.18 min for MPA and IS, respectively. The lower limit of quantification of MPA was 0.1 μg/ml. The within- and between-assay reproducibility results ranged from 1.81 to 10.72%. Patient and external quality assessment sample results were comparable with those obtained previously by an in-house validated LC-MS/MS method. This method showed satisfactory analytical performance for the determination of MPA in plasma over the calibration range of 0.1-15.0 μg/ml. |
| Databáze: | OpenAIRE |
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