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Validation and application of a liquid chromatography‐tandem mass spectrometric method for the determination of GDC‐0152 in human plasma using solid‐phase extraction
Author(s) -
Shin Young G.,
Jones Steve A.,
Murakami Stan C.,
Budha Nageshwar,
Ware Joseph,
Wong Harvey,
Buonarati Michael H.,
Dean Brian,
Hop Cornelis E. C. A.
Publication year - 2013
Publication title -
biomedical chromatography
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 0.4
H-Index - 65
eISSN - 1099-0801
pISSN - 0269-3879
DOI - 10.1002/bmc.2754
Subject(s) - chemistry , chromatography , extraction (chemistry) , calibration curve , human plasma , sample preparation , solid phase extraction , detection limit , tandem mass spectrometry , liquid chromatography–mass spectrometry , analytical chemistry (journal) , mass spectrometry
A liquid chromatography–tandem mass spectrometric (LC‐MS/MS) method was developed and validated for the determination of GDC‐0152 in human plasma to support clinical development. The method consisted of a solid‐phase extraction for sample preparation and LC‐MS/MS analysis in the positive ion mode using TurboIonSpray TM for analysis. d 7 ‐GDC‐0152 was used as the internal standard. A linear regression (weighted 1/concentration 2 ) was used to fit calibration curves over the concentration range of 0.02–10.0 ng/mL for GDC‐0152. There were no endogenous interference components in the blank human plasma tested. The accuracy at the lower limit of quantitation was 99.3% with a precision (%CV) of 13.9%. For quality control samples at 0.0600, 2.00 and 8.00 ng/mL, the between‐run %CV was ≤8.64. Between‐run percentage accuracy ranged from 98.2 to 99.6%. GDC‐0152 was stable in human plasma for 363 days at −20°C and for 659 days at −70°C storage. GDC‐0152 was stable in human plasma at room temperature for up to 25 h and through three freeze–thaw cycles. In whole blood, GDC‐0152 was stable for 12 h at 4°C and at ambient temperature. This validated LC‐MS/MS method for determination of GDC‐0152 was used to support clinical studies. Copyright © 2012 John Wiley & Sons, Ltd.