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.
Subject(s)
Chromatography, High Pressure Liquid/methods , Serotonin Receptor Agonists/blood , Spectrometry, Mass, Electrospray Ionization/methods , Sumatriptan/blood , Administration, Intranasal , Area Under Curve , Humans , Male , Sensitivity and Specificity , Serotonin Receptor Agonists/administration & dosage , Serotonin Receptor Agonists/pharmacokinetics , Sumatriptan/administration & dosage , Sumatriptan/pharmacokineticsABSTRACT
A sensitive and convenient high-performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS) assay for the opioid receptor agonist-antagonist butorphanol in human plasma is described. BC-2605, a cyclopropyl analogue of butorphanol, was employed as an internal standard. Butorphanol was recovered from plasma (84.4 +/- 10.9%) 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 microm). The standard curve was linear from 13.7 to 1374 pg/ml (r(2)>0.99). The lower limit of quantitation was 13.7 pg/ml. The assay was specific, accurate (% deviation from nominal concentrations were <15%), precise and reproducible (within- and between-day coefficients of variation <7%). Butorphanol in plasma was stable over 3 freeze/thaw cycles and at room temperature for 1 day. The utility of the assay was demonstrated by following butorphanol plasma concentrations in two healthy subjects for 24 h following a 1 mg intranasal dose.
