title: Validation and application of a high-performance liquid chromatography/tandem mass spectrometry assay for sumatriptan in human plasma.
abstract: A sensitive and convenient high-performance liquid chromatography-tandem mass spectrometry(HPLC-MS/MS) assay is described for the (5-HT(lB/lD)) receptor agonist sumatriptan in human plasma. Sumatriptan was recovered from plasma (81.8 +/- 6.8%) by liquid-liquid extraction. The mobile phase flow rate was 0.3 mL/min and consisted of methanol:water:formic acid (90:10:0.1, v/v/v). The analytical column (4.6 x 100 mm) was packed with Partisil C(8) (5 micro m). The standard curve was linear from 0.7 to 70.4 ng/mL (r(2) > 0.99). The lower limit of quantitation was 0.7 ng/mL. The assay was specific, accurate (percentage deviation from nominal concentrations were <15%), precise and reproducible (within- and between-day coefficients of variation <10.3%). Sumatriptan in plasma was stable over three freeze/thaw cycles and at room temperature for one day. The utility of the assay was demonstrated by following sumatriptan plasma concentrations in two healthy subjects for 8-12 h following a single 20 mg intranasal dose.
authors.affiliation: Clinical Discovery, Bristol-Myers Squibb Pharmaceutical Research Institute, Princeton, NJ 08543, USA. david.boulton@bms.com
authors.forename: David W
authors.initials: DW
authors.lastname: Boulton
authors.forename: Glenn F
authors.initials: GF
authors.lastname: Duncan
authors.forename: Nimish N
authors.initials: NN
authors.lastname: Vachharajani
mesh_terms: D000281:Administration, Intranasal; D019540:Area Under Curve; D002851:Chromatography, High Pressure Liquid / Q000379:methods*; D006801:Humans; D008297:Male; D012680:Sensitivity and Specificity; D017366:Serotonin Receptor Agonists / Q000008:administration & dosage / Q000097:blood* / Q000493:pharmacokinetics; D021241:Spectrometry, Mass, Electrospray Ionization / Q000379:methods*; D018170:Sumatriptan / Q000008:administration & dosage / Q000097:blood* / Q000493:pharmacokinetics
chemical_list: D017366:Serotonin Receptor Agonists; D018170:Sumatriptan