title: Simple and rapid determination of norethindrone in human plasma by supported liquid extraction and ultra performance liquid chromatography with tandem mass spectrometry.
abstract: We report for the first time an ultra performance liquid chromatographic method with tandem mass spectrometric detection (UPLC/MS/MS) for the determination of norethindrone alone in human plasma over the concentration range of 50.0-25000 pg mL(-1) using a sample volume of 0.250 mL. Norethindrone and its internal standard (ISTD), norethindrone-(13)C(2), were extracted from human plasma by supported liquid extraction (SLE). After evaporation of the organic solvent, samples were reconstituted and analyzed on an UPLC/MS/MS system. The UPLC system used a Waters BEH C18 (100 mm × 2.1mm, 1.7 μm) column with mobile phase A of 0.05% formic acid in water:acetonitrile (65:35, v/v) and mobile phase B of 0.05% formic acid in methanol:acetonitrile (50:50, v/v). The flow rate was 0.500 mL min(-1). The method was fully validated. The inter-run accuracy and precision at the lower limit of quantitation (LLOQ), low, mid and high quality control (QC) concentration levels were 99.2-108.4% with a <8.1% CV (coefficient of variation), respectively. The validated method has been successfully applied to analysis of thousands of pharmacokinetic samples.
authors.affiliation: Department of Bioanalytical Chemistry, Covance Inc., 8211 SciCor Dr., Indianapolis, IN 46214, USA. zhilong.gong@covance.com
authors.forename: Zhilong
authors.initials: Z
authors.lastname: Gong
authors.forename: Kiresha
authors.initials: K
authors.lastname: Chandler
authors.forename: Stephen
authors.initials: S
authors.lastname: Webster
authors.forename: Remy
authors.initials: R
authors.lastname: Kerley
authors.forename: Susan
authors.initials: S
authors.lastname: Buist
authors.forename: Melanie
authors.initials: M
authors.lastname: McCort-Tipton
mesh_terms: D002851:Chromatography, High Pressure Liquid / Q000379:methods; D006801:Humans; D057230:Limit of Detection; D009640:Norethindrone / Q000097:blood*; D015203:Reproducibility of Results; D053719:Tandem Mass Spectrometry / Q000379:methods*
chemical_list: D009640:Norethindrone