Determination of PF-04928473 in human plasma using liquid chromatography with tandem mass spectrometry.
J Chromatogr B Analyt Technol Biomed Life Sci
; 878(30): 3187-92, 2010 Nov 15.
Article
em En
| MEDLINE
| ID: mdl-20951100
ABSTRACT
A simple, rapid and sensitive liquid chromatography/tandem mass spectrometric (LC/MS/MS) analytical method was developed for quantification of Hsp90 inhibitor PF-04928473 in human plasma, following administration of its prodrug, PF-04929113. Sample processing involved protein precipitation by addition of 0.4 mL of methanol containing internal standard (PF-04972487) to 50 µL volume of plasma sample. Chromatographic separation of PF-04928473 and PF-04972487 was achieved on a Phenomenex®) Luna C18(2) (2.0 mm x 50 mm, 5 µm) column using a gradient elution method with mobile phase solvents methanol containing 0.1% formic acid and 0.1% formic acid at a flow rate of 0.25 mL/min. Detection was performed in electrospray positive ionization mode, monitoring the ion transitions from m/z 465.1â350.1 (PF-04928473) and m/z 447.0â329.1 (PF-04972487). The retention times for PF-04928473 and PF-04972487 were 1.86 and 2.85 min, respectively. Calibration curves were generated in the range of 2-2000 ng/mL. The accuracy and precision ranged from 94.1 to 99.0% and 86.7 to 97.6%, respectively, which were calculated using quality control samples of three different concentrations analyzed in quintuplicate on four different days.
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Base de dados:
MEDLINE
Assunto principal:
Cromatografia Líquida de Alta Pressão
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Proteínas de Choque Térmico HSP90
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Espectrometria de Massas em Tandem
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Compostos Heterocíclicos de 4 ou mais Anéis
Idioma:
En
Ano de publicação:
2010
Tipo de documento:
Article