Simultaneous determination of sivelestat and its metabolite XW-IMP-A in human plasma using HPLC-MS/MS / 药学学报
Acta Pharmaceutica Sinica
;
(12): 1318-1323, 2015.
Article
in Chinese
| WPRIM
| ID: wpr-320083
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.
Full text:
Available
Index:
WPRIM (Western Pacific)
Main subject:
Sulfonamides
/
Blood
/
Reproducibility of Results
/
Chromatography, High Pressure Liquid
/
Chromatography, Liquid
/
Tandem Mass Spectrometry
/
Glycine
/
Inosine Monophosphate
Type of study:
Prognostic study
Limits:
Humans
Language:
Chinese
Journal:
Acta Pharmaceutica Sinica
Year:
2015
Type:
Article
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