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Application of a UPLC‐MS/MS method for the analysis of alosetron in human plasma to support a bioequivalence study in healthy males and females
Author(s) -
Chaudhary Darshan V.,
Patel Daxesh P.,
Shah Jaivik V.,
Shah Priyanka A.,
Sanyal Mallika,
Shrivastav Pranav S.
Publication year - 2015
Publication title -
biomedical chromatography
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 0.4
H-Index - 65
eISSN - 1099-0801
pISSN - 0269-3879
DOI - 10.1002/bmc.3454
Subject(s) - chromatography , formic acid , chemistry , ammonium formate , high performance liquid chromatography , bioequivalence , analyte , selected reaction monitoring , solid phase extraction , extraction (chemistry) , mass spectrometry , tandem mass spectrometry , liquid chromatography–mass spectrometry , analytical chemistry (journal) , pharmacokinetics , medicine , pharmacology
A simple, rapid and sensitive ultra‐performance liquid chromatography–tandem mass spectrometry (UPLC‐MS/MS) method has been developed and validated for the determination of alosetron (ALO) in human plasma. The assay method involved solid‐phase extraction of ALO and ALO 13C‐d3 as internal standard (IS) on a LichroSep DVB‐HL (30 mg, 1 cm 3 ) cartridge. The chromatography was performed on an Acquity UPLC BEH C 18 (50 × 2.1 mm, 1.7 µm) column using acetonitrile and 2.0 m m ammonium formate, pH 3.0 adjusted with 0.1% formic acid (80:20, v/v) as the mobile phase in an isocratic mode. For quantitative analysis, the multiple reaction monitoring transitions studied were m/z 295.1/201.0 for ALO and m/z 299.1/205.1 for IS in the positive ionization mode. The method was validated over a concentration range of 0.01–10.0 ng/mL for ALO. Post‐column infusion experiment showed no positive or negative peaks in the elution range of the analyte and IS after injection of extracted blank plasma. The extent of ion‐suppression/enhancement, expressed as IS‐normalized matrix factor, varied from 0.96 to 1.04. The assay recovery was within 97–103% for ALO and IS. The method was successfully applied to support a bioequivalence study of 1.0 mg alosetron tablets in 28 healthy Indian male and female subjects. Copyright © 2015 John Wiley & Sons, Ltd.