RESUMEN
A specific and reliable HPLC-MS/MS method was developed and validated for the simultaneous determination of six alkaloids in rat plasma, jatrorrhizine, berberine, tetrahydropalmatine, protopine, bicuculline and palmatine. The analytes were separated on a C18 column (50mm×2.1mm, 1.8µm) and a triple-quadrupole mass spectrometry equipped with an electrospray ionization (ESI) source was used for detection. The plasma sample was prepared by the simple protein precipitation and the recovery for the six analytes was over 80%. The calibration curves were linear over a concentration range of 0.38-1900.0ng/mL for jatrorrhizine, 0.57-2850.0ng/mL for berberine, 0.32-1600.0ng/mL for tetrahydropalmatine, 0.21-1050.0ng/mL for protopine, 0.34-1700.0ng/mL for bicuculline and 0.22-1100ng/mL for palmatine. The intra-day and inter-day precision was less than 15% and the relative error (RE) was all within ±15%. The validated method was successfully applied to a pharmacokinetics study in rats after oral administration of the extracts of Rhizoma Corydalis Decumbentis (a famous Chinese herb).
Asunto(s)
Alcaloides/sangre , Cromatografía Líquida de Alta Presión/métodos , Corydalis/química , Rizoma/química , Espectrometría de Masas en Tándem/métodos , Alcaloides/química , Alcaloides/aislamiento & purificación , Alcaloides/farmacocinética , Animales , Modelos Lineales , Masculino , Extractos Vegetales/administración & dosificación , Extractos Vegetales/química , Ratas , Ratas Sprague-Dawley , Reproducibilidad de los Resultados , Sensibilidad y EspecificidadRESUMEN
A specific and reliable HPLC-MS/MS method was developed and validated for the determination of ara-U in human plasma. The analyte was separated on a C18 column (50 mm × 2.1mm, 1.7 µm) and a triple-quadrupole mass spectrometry equipped with an electrospray ionization (ESI) source was applied for detection. The plasma sample was prepared by a simple protein precipitation pretreatment and the recovery was about 80%. The calibration curves were linear over a concentration range of 1.0-7000.0 ng/mL for ara-U. The intra-day and inter-day precision was less than 15% and the relative error (RE) was all within ± 15%. It was successfully applied to assess the disposition characteristics of ara-U and support the therapeutic drug monitoring after the patients with leukemia were infused with ara-C.
Asunto(s)
Arabinofuranosil Uracilo/sangre , Cromatografía Líquida de Alta Presión/métodos , Monitoreo de Drogas/métodos , Leucemia/tratamiento farmacológico , Espectrometría de Masas en Tándem/métodos , Calibración , Humanos , Espectrometría de Masa por Ionización de ElectrosprayRESUMEN
A simple and sensitive HPLC-MS/MS method was developed and validated for the simultaneous determination of decitabine and valdecitabine in rat plasma. The analytes were separated on a C(18) column (150mm×4.6mm, 3.5µm) and a triple-quadrupole mass spectrometer equipped with an electrospray ionization (ESI) source was applied for detection. A clean solid-phase extraction procedure with cation exchange cartridge was employed to extract the analytes from rat plasma with high recovery of decitabine (>82%). The calibration curves were linear over a concentration range of 10-10,000ng/mL for decitabine and 5-500ng/mL for valdecitabine. The lower limit of quantitation (LLOQ) of decitabine and valdecitabine was 10 and 5ng/mL, respectively. The intra-day and inter-day precisions were less than 15% and the relative error (RE) was all within ±15%. The validated method was successfully applied to a pharmacokinetics study in rats after either decitabine or valdecitabine orally administrated to the Sprague-Dawley rats.
