RESUMEN
A sensitive and specific liquid chromatographic-tandem mass spectrometric (LC-MS-MS) method has been validated for the measurement of YF476 in human plasma. The method involves a simple liquid-liquid extraction procedure, chromatography of the extracts on a C(18) column, atmospheric pressure chemical ionisation and detection in the multiple reaction monitoring mode. The calibration line was linear over the concentration range 0.1 ng/ml (the limit of quantification) to 25.0 ng/ml. Intra- and inter-batch precision was <14% and intra- and inter-batch accuracy was <11% over the entire calibration range. The bioanalytical method is robust and has been used for the analysis of many samples from human subjects involved in early clinical studies (Phase I).
Asunto(s)
Benzodiazepinonas/sangre , Antagonistas de Hormonas/sangre , Compuestos de Fenilurea/sangre , Animales , Benzodiazepinonas/farmacocinética , Calibración , Perros , Semivida , Antagonistas de Hormonas/farmacocinética , Humanos , Compuestos de Fenilurea/farmacocinética , Ratas , Reproducibilidad de los Resultados , Sensibilidad y EspecificidadRESUMEN
A liquid chromatographic tandem mass spectrometric method for the quantitative determination of sumatriptan base in human plasma and urine has been developed and validated over the concentration range 0.2-20 ng base ml-1. Sumatriptan is a 5-HT1 receptor agonist which has found widespread use in the treatment of migraine. Sumatriptan and its internal standard (D3-sumatriptan) were extracted from human matrices using C2 solid phase cartridges. The extracts were chromatographed on a C18 column, ionised using a heated nebuliser assisted atmospheric pressure ionisation (API) interface and detected by MS/MS in the multiple reaction monitoring mode. The completed validation demonstrated the method to be robust, accurate, precise and specific for the direct quantification of sumatriptan in human fluids. The method was used on a routine basis to determine the levels of sumatriptan in human volunteers following the oral administration of a 25 mg dose of sumatriptan succinate.
Asunto(s)
Cromatografía Liquida/métodos , Espectrometría de Masas/métodos , Sumatriptán/sangre , Sumatriptán/orina , Estabilidad de Medicamentos , Estudios de Evaluación como Asunto , Humanos , Espectrometría de Masas/instrumentación , Estándares de Referencia , Sumatriptán/químicaRESUMEN
The technique of fast atom bombardment mass spectrometry has been shown to be capable of producing molecular weight and useful fragmentation information from a selection of penicilloic acids. In addition, the technique has been shown to give similar information on alkali metal salts of penicilloic acids.