title: Determination of Simvastatin in human plasma by liquid chromatography-mass spectrometry.
abstract: A simple, sensitive and selective liquid chromatography coupled with electrospray ionization mass spectrometry (LC/ESI/MS) method for the determination of simvastatin (I) has been developed. After extraction by ethyl acetate, using lovastatin (II) as internal standard, solutes are separated on a C(18) column with a mobile phase consisting of methanol-water (9:1). Detection is performed on an atmospheric pressure ionization single quadruple mass spectrometer equipped with an ESI interface and operates in positive ionization mode. Simvastatin quantification was realized by computing peak area ratio (I/II) of the extracts analyzed in SIM mode (m/z: 441 and m/z: 427 for I and II, respectively) and comparing them with calibration curve (r=0.9997). Accuracy and precision for the assay were determined by calculating the intra-batch and inter-batch variation at three concentrations 0.1, 5.0, 10.0 ng/ml; the intra batch relative standard deviation (RSD) was less than 10% and ranged from 1.8 to 8.5%, respectively; the inter-batch RSD was less than 20% and ranged from 4.1 to 16.5%. The limit of detection was 0.05 ng/ml.
authors.affiliation: Laboratory of R&D, Nanjing Kangxing Pharmaceutical Ltd, Nanjing, China. htyang2000@yahoo.com
authors.forename: Haitao
authors.initials: H
authors.lastname: Yang
authors.forename: Yan
authors.initials: Y
authors.lastname: Feng
authors.forename: Yiwen
authors.initials: Y
authors.lastname: Luan
mesh_terms: D000328:Adult; D002138:Calibration; D002853:Chromatography, Liquid; D018592:Cross-Over Studies; D017022:Flow Injection Analysis; D006801:Humans; D019161:Hydroxymethylglutaryl-CoA Reductase Inhibitors / Q000097:blood* / Q000493:pharmacokinetics; D008148:Lovastatin / Q000097:blood; D000432:Methanol / Q000737:chemistry; D011786:Quality Control; D012015:Reference Standards; D015203:Reproducibility of Results; D019821:Simvastatin / Q000097:blood* / Q000493:pharmacokinetics; D012996:Solutions; D012997:Solvents; D021241:Spectrometry, Mass, Electrospray Ionization
chemical_list: D019161:Hydroxymethylglutaryl-CoA Reductase Inhibitors; D012996:Solutions; D012997:Solvents; D008148:Lovastatin; D019821:Simvastatin; D000432:Methanol