Development and validation of a liquid chromatographic-mass spectrometric assay for the determination of sumatriptan in plasma.
Sumatriptan succinate is a novel compound currently in development for the acute treatment of migraine. During early studies in man a sensitive and selective assay was required, which had to be developed rapidly, to determine plasma concentrations following an intravenous infusion. Thermospray liquid chromatography-mass spectrometry combined with the advanced automated sample processor was selected to achieve this. Although the assay was required quickly criteria for intra- and inter-assay accuracies and precisions of +/- 10% had to be achieved. These were obtained only by using a co-eluting deuterium-labelled internal standard. Attempts to use a homologue as an internal standard, which did not co-elute with sumatriptan, gave inferior results. The assay was linear over the calibration range 2-50 ng/ml with a limit of quantification of 2 ng/ml. The application of the technique to the analysis of samples from a volunteer study is demonstrated.
Oxford
J
J
Biochemical Pharmacology Division, Glaxo Group Research Limited, Ware, Hertfordshire, U.K.
Lant
M S
MS
D055598:Chemical Phenomena; D002621:Chemistry; D002853:Chromatography, Liquid / Q000379:methods; D006801:Humans; D007211:Indoles / Q000097:blood*; D013058:Mass Spectrometry / Q000379:methods; D008881:Migraine Disorders / Q000188:drug therapy*; D013449:Sulfonamides / Q000097:blood*; D018170:Sumatriptan
D007211:Indoles; D013449:Sulfonamides; D018170:Sumatriptan