Quantitative determination of nebivolol from human plasma using liquid chromatography-tandem mass spectrometry
| Autor: | S.J. Rajput, Pritesh Contractor, Mohsin Vohra, Bhavik Solanki, Jatin Nandania, Pragnesh Vasava |
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| Rok vydání: | 2012 |
| Předmět: |
Adult
Male Analyte Clinical Biochemistry Analytical chemistry Ion suppression in liquid chromatography–mass spectrometry Mass spectrometry Biochemistry High-performance liquid chromatography Sensitivity and Specificity Analytical Chemistry Nebivolol Drug Stability Liquid chromatography–mass spectrometry Tandem Mass Spectrometry Humans Benzopyrans Chromatography Cross-Over Studies Chemistry Selected reaction monitoring Reproducibility of Results Cell Biology General Medicine Triple quadrupole mass spectrometer Therapeutic Equivalency Ethanolamines Linear Models Female Stock solution Chromatography Liquid |
| Zdroj: | Journal of chromatography. B, Analytical technologies in the biomedical and life sciences. |
| ISSN: | 1873-376X |
| Popis: | In the present work, a rapid, sensitive, specific, precise and accurate liquid chromatography-tandem mass spectrometry method for determination of nebivolol in human plasma was developed and validated with a large calibration curve range (50-5000 pg/mL) which can be used for routine drug analysis and bioequivalence studies. Liquid-liquid extraction method was used to extract the analyte from the human plasma. The separation was achieved using Waters symmetry, C18, 4.6 × 150 mm, 5 μm column with formic acid in water, 0.01%, v/v: Acetonitrile (40:60) as a mobile phase. A flow rate of 0.8 mL/min, no splitting and run time 2.00 min was used for the chromatographic analysis of nebivolol. Sensitivity of this method was found to be 30 pg/mL. The analyte was analyzed by mass spectrometry in the multiple reaction monitoring mode. A Turbo-Ion spray source was interfaced between the HPLC and triple quadrupole mass spectrometer (MDS Sciex API 4000). The precursor-product ion m/z 406.00-151.00 for nebivolol and m/z 410.20-151.00 for nebivolol-D4 were used for quantification of an analyte and its IS. The method was validated in terms of accuracy, precision, selectivity, absolute recovery, freeze-thaw stability, bench-top stability, dry extract stability, short and long term stock solution stability, wet extract stability and re-injection reproducibility. The within- and between-batch accuracy was found to lie within the range of 87.00-100.40% and within- and between-batch precision was obtained within the range 0.33-8.67%. The mean recovery of all three concentration levels for drug was obtained 67.67% where as the mean recovery of IS was 68.74%. The %RSD value at higher concentration and lower concentration in all stability experiments was within 15%. This method is free from ion suppression, ion enhancement and any type of abnormal ionization. |
| Databáze: | OpenAIRE |
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