Determination of Some Drugs in Blood Plasma Using Liquid Chromatography-MS

Qasim Mezban  Salih

Qasim Mezban Salih College of Science, Wasit University, Wasit, Iraq

Keywords: spectrometry, febuxostat human plasma, bioequivalence, chromatography

Abstract

The accurate quantification regarding febuxostat levels in human plasma will be accomplished using a liquid chromatography - tandem mass spectrometry (LCESI-MS/MS) assay with a robust sensitivity, selectivity, and reliability. Indomethacin was used as the internal standard (IS) in the test. Using methyl tert-butyl ether as extraction solvent, the analyte as well as IS have been mined from 200μL human plasma sample using extraction procedure (liquid - liquid). A Hypurity C-18 column with particle size dimensions of 100mm x 4.6mm and a column with 5μm particle size were used in the experiment in order to perform the chromatography. Under isocratic circumstances, the chromatography has been performed. Tandem mass spectrometry, which could operate in a negative ionization reaction condition range and efficiently observe various reaction modes, has been used for the purpose of detecting the analyte and internal standard. The deprotonated precursor ions were represented by observed changes of product ions for the febuxostat and indomethacin, which have been m/z 356.10 → 312 and 315.10 → 271, respectively. This technique had demonstrated a 0.05μg/mL limit of quantitation and a 0.0025 μg/mL limit of detection. Validated linear dynamic range of febuxostat has been found to be 0.05g/mL–6g/mL. Precision, which is expressed as the coefficient of variation (% CV) within and across batches, has been determined to be ≤7.1%. It was revealed that average extraction recovery of the febuxostat at various levels of quality control has been >87%. In order to ascertain bio-equivalence of 80mg febuxostat tablet form in a group that includes 14 healthy males of origin, the current study successfully used the previously indicated methodology. The experiment was conducted under both fed and fasted circumstances. The potential for duplicating the measurements regarding study outcomes was shown by re-examining 110 incurred cases.

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