Validation and application of a liquid chromatography‐tandem mass spectrometric method for the determination of GDC‐0152 in human plasma using solid‐phase extraction |
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Authors: | Young G. Shin Steve A. Jones Stan C. Murakami Nageshwar Budha Joseph Ware Harvey Wong Michael H. Buonarati Brian Dean Cornelis E. C. A. Hop |
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Affiliation: | 1. Department of Drug Metabolism and Pharmacokinetics, Genentech, , South San Francisco, CA, 94080 USA;2. Intertek‐Alta Analytical Laboratory, , El Dorado Hills, CA, 95762 USA |
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Abstract: | 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 TurboIonSprayTM for analysis. d7‐GDC‐0152 was used as the internal standard. A linear regression (weighted 1/concentration2) 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. |
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Keywords: | GDC‐0152 LC‐MS/MS human plasma validation |
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