Addressing the need for biomarker liquid chromatography/mass spectrometry assays: A protocol for effective method development for the bioanalysis of endogenous compounds in cerebrospinal fluid

2013 ◽  
Vol 27 (16) ◽  
pp. 1882-1886 ◽  
Author(s):  
Yulia Benitex ◽  
Colleen A. McNaney ◽  
David Luchetti ◽  
Eric Schaeffer ◽  
Timothy V. Olah ◽  
...  
Keyword(s):  
Mass Spectrometry ◽  
Cerebrospinal Fluid ◽  
Liquid Chromatography ◽  
Method Development ◽  
Liquid Chromatography Mass Spectrometry ◽  
Chromatography Mass Spectrometry ◽  
Endogenous Compounds

scholarly journals NEW METHOD DEVELOPMENT AND VALIDATION FOR THE DETERMINATION OF FEBUXOSTAT IN HUMAN PLASMA BY LIQUID CHROMATOGRAPHY–MASS SPECTROMETRY

2016 ◽  
Vol 8 (9) ◽  
pp. 61 ◽  
Author(s):  
Narottam Pal ◽  
Avanapu Srinivasa Rao ◽  
Pigilli Ravikumar
Keyword(s):  
Mass Spectrometry ◽  
Liquid Chromatography ◽  
Human Plasma ◽  
Method Development ◽  
Multiple Reaction Monitoring ◽  
Internal Standard ◽  
New Method ◽  
Liquid Chromatography Mass Spectrometry ◽  
Chromatography Mass Spectrometry

<p><strong>Objective</strong>:<strong> </strong>To develop a new method and validate the same for the determination of Febuxostat (FBS) in human plasma by liquid chromatography–mass spectrometry (LCMS).</p><p><strong>Methods</strong>:<strong> </strong>The present method utilized reversed-phase high-performance liquid chromatography with tandem mass spectroscopy. Febuxostat D9 (FBS D9) was used as internal standard (IS). The analyte and internal standard were separated from human plasma by using solid phase extraction method. Zorbax Eclipse XDB, C<sub>8</sub>, 100 mm x 4.6 mm, 3.5 µm column was used and HPLC grade acetonitrile, 5 millimolar (mM) ammonium format (80: 20, v/v) as mobile phase, detected by mass spectrometry operating in positive ion and multiple reaction monitoring modes.</p><p><strong>Results</strong>:<strong> </strong>The parent and production transitions for FBS and internal standard were at m/z 317.1→261.0 and 326.1→262.0 respectively. The method was validated for system suitability, specificity, carryover effect, linearity, precision, accuracy, matrix effect, sensitivity and stability. The linearity range was from 20.131 ng/ml to10015. 534 ng/ml with a correlation coefficient of 0.999. Precision results (%CV) across six quality control samples were within the limit. The percentage recovery of FBS and internal standard from matrix samples was found to be 76.57% and 75.03% respectively.</p><p><strong>Conclusion</strong>:<strong> </strong>Present study describes new LC-MS method for the quantification of FBS in a pharmaceutical formulation. According to validation results, it was found to be a simple, sensitive, accurate and precise method and also free from any kind of interference. Therefore the proposed analytical method can be used for routine analysis for the estimation of FBS in its formulation.</p>

scholarly journals A HIGH-PERFORMANCE LIQUID CHROMATOGRAPHY–MASS SPECTROMETRY/MASS SPECTROMETRY METHOD DEVELOPMENT FOR THE QUANTITATIVE DETERMINATION OF BISOPROLOL FROM CACO-2 CELL MONOLAYERS

2018 ◽  
Vol 11 (4) ◽  
pp. 386
Author(s):  
Liliya Logoyda ◽  
Dmytro Korobko
Keyword(s):  
Mass Spectrometry ◽  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
High Performance ◽  
Method Development ◽  
Sample Volume ◽  
Liquid Chromatography Mass Spectrometry ◽  
Cell Monolayers ◽  
Chromatography Mass Spectrometry

 Objective: A simple, rapid high-performance liquid chromatography–mass spectrometry (MS)/MS method was developed for the determination of bisoprolol from confluent Caco-2 monolayers and from aqueous solution.Methods: Chromatography was achieved on discovery C 18, 50 mm×2.1 mm, 5 μm column. Samples were chromatographed in a gradient mode (eluent A [acetonitrile:water:formic acid, 5:95:0.1 v/v] and eluent B [acetonitrile:formic acid, 100:0.1 v/v]). The initial content of the eluent B is 0%, which increases linearly by 1.0 min to 100% and to 1.01 min returns to the initial 0%. The mobile phase was delivered at a flow rate of 0.400 ml/min into the mass spectrometer ESI chamber. The sample volume was 5 μl.Results: Under these conditions, bisoprolol was eluted at 1.49 min. According to the Caco-2 test results, bisoprolol appeared to have moderate to high permeability. It should be noted that the recovery value for bisoprolol is 97.69%. Caco-2 permeability values for bisoprolol are in agreement with BCS Class I classification for these drugs and their known high bioavailability in humans.Conclusion: From results of analysis, it can be concluded that developed method is simple and rapid for the determination of bisoprolol from confluent Caco-2 monolayers and from aqueous solution. Acquired results demonstrate that proposed strategy can be effortlessly and advantageously applied for the examination of bisoprolol from Caco-2 cell monolayers.

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