Evaluation of dried blood spot (DBS) technology versus plasma analysis for the determination of MK-1775 by HILIC-MS/MS in support of clinical studies

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• 作者：Yang Xu (1)
  Wei Fang (1)
  Wei Zeng (1)
  Suzanne Leijen (2)
  Eric J. Woolf (1)
  
• 关键词：MK ; 1775 ; Dried blood spot (DBS) ; Hematocrit impact ; Hydrophilic interaction liquid chromatography (HILIC) ; Tandem mass spectrometry (MS/MS) ; Blood ; to ; plasma (B/P) ratio
• 刊名：Analytical and Bioanalytical Chemistry
• 出版年：2012
• 出版时间：December 2012
• 年：2012
• 卷：404
• 期：10
• 页码：3037-3048
• 全文大小：438KB
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• 作者单位：Yang Xu (1)
  Wei Fang (1)
  Wei Zeng (1)
  Suzanne Leijen (2)
  Eric J. Woolf (1)
  
  1. Department of Pharmacokinetics, Pharmacodynamics and Drug Metabolism, Regulated Bioanalysis, Merck Research Laboratories, WP75B-300, West Point, PA, 19486, USA
  2. Department of Clinical Pharmacology & Molecular Pathology, The Netherlands Cancer Institute, 1066 CX, Amsterdam, The Netherlands
  
• ISSN：1618-2650

文摘

The collection of human blood samples as dried blood spots (DBS) for the pharmacokinetic assessment of investigational drugs in clinical trials offers a number of advantages over conventional plasma sampling, namely, small sample volume, simplified sample handling, and cost-effective shipping and storage. The use of DBS coupled with liquid chromatography–tandem mass spectrometry analysis was evaluated for the quantification of MK-1775, a Wee-1 inhibitor under development as a chemo/radio-sensitizer for the treatment of cancer. The DBS method exhibited an assay performance comparable to that of the existing plasma assay, which is currently used in support of clinical studies. Both assays used the same linear dynamic range of 2-,000?ng/mL, with a lower limit of quantification of 2?ng/mL. Based on the intra-day assay validation results, the accuracy of the DBS method ranged from 94.0 to 105.0?%, with a coefficient of variation of <4.8?%. The blood-to-plasma ratio calculated from the DBS data (blood concentrations) and the plasma data (plasma concentrations) was in good agreement with the one obtained from the in vitro assessment using conventional methodology. No significant hematocrit impact on the assay was observed as hematocrit ranged from 16 to 85?%. The correlation between the measured MK-1775 concentrations in plasma and that determined in dried blood spots from oncology patients during the ongoing clinical study was discussed.