title: [Simultaneous determination of sivelestat and its metabolite XW-IMP-A in human plasma using HPLC-MS/MS].
abstract: A simple and rapid method was developed based on high performance liquid chromatography coupled to tandem mass spectrometry (LC-MS/MS) to determine sivelestat and its metabolite XW-IMP-A in human plasma. After a simple protein precipitation, the samples and internal standards were analyzed on a C18 column by a gradient elution program. The mobile phase consisted of 30% acetonitrile in methanol and 5 mmol · L(-1) ammonium acetate at a flow rate of 0.7 mL · min(-1). The mass spectrometric data was collected in multiple reaction monitoring mode (MRM) in the negative electrospray ionization. The standard curves were linear in the range of 10.0-15,000 ng · mL(-1) for sivelestat, and 2.50-1000 ng · mL(-1) for XW-IMP-A. The low limits of quantitation were identified at 10.0 and 2.50 ng · mL for sivelestat and XW-IMP-A, respectively. The intra- and inter-day precision were within 11.3% and 13.1% for sivelestat and XW-IMP-A, and accuracy was 0.3% and 0.6% for sivelestat and XW-IMP-A, within the acceptable limits across all concentrations. The method was successfully validated in the pharmacokinetic study of sivelestat in healthy Chinese volunteers.
authors.forename: Jing
authors.initials: J
authors.lastname: Wang
authors.forename: Xiao-jian
authors.initials: XJ
authors.lastname: Dai
authors.forename: Yi-fan
authors.initials: YF
authors.lastname: Zhang
authors.forename: Da-fang
authors.initials: DF
authors.lastname: Zhong
authors.forename: Yu-lin
authors.initials: YL
authors.lastname: Wu
authors.forename: Xiao-yan
authors.initials: XY
authors.lastname: Chen
mesh_terms: D002851:Chromatography, High Pressure Liquid; D002853:Chromatography, Liquid; D005998:Glycine / Q000031:analogs & derivatives* / Q000097:blood; D006801:Humans; D007291:Inosine Monophosphate / Q000097:blood*; D015203:Reproducibility of Results; D013449:Sulfonamides / Q000097:blood*; D053719:Tandem Mass Spectrometry
chemical_list: D013449:Sulfonamides; D007291:Inosine Monophosphate; C069195:sivelestat; D005998:Glycine