Determination of CC-5013, an analogue of thalidomide, in human plasma by liquid chromatography-mass spectrometry

Tanyifor M. Tohnya, Kyunghwa Hwang, Erin R. Lepper, Howard A. Fine, William L. Dahut, Jürgen Venitz, Alex Sparreboom, William D. Figg

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A high-performance liquid chromatographic assay with MS detection has been developed for the quantitative determination of the anti-angiogenic agent CC-5013 in human plasma. Sample pretreatment involved liquid-liquid extraction with acetonitrile/1-chlorobutane (4:1, v/v) solution containing the internal standard, umbelliferone. Separation of the compounds of interest was achieved on a column packed with Waters C18 Nova-Pak material (4 μm particle size; 300 mm × 3.9 mm internal diameter) using acetonitrile, de-ionized water, and glacial acetic acid in ratios of 20:80:0.1 (v/v/v) (pH 3.5) delivered at an isocratic flow rate of 1.00 ml/min. Simultaneous MS detection was performed at m/z 260.3 (CC-5013) and m/z 163.1 (umbelliferone). The calibration curve was fit to a linear response-concentration data over a range of 5-1000 ng/ml using a weighting factor of 1/x. Values for accuracy and precision, obtained from four quality controls analyzed on three different days in replicates of five, ranged from 98 to 106% and from 5.5 to 15.5%, respectively. The method was successfully applied to study the pharmacokinetics of CC-5013 in a cancer patient receiving the drug as single daily dose.

Original languageEnglish
Pages (from-to)135-141
Number of pages7
JournalJournal of Chromatography B: Analytical Technologies in the Biomedical and Life Sciences
Issue number2
StatePublished - 25 Nov 2004
Externally publishedYes


  • Angiogenesis inhibitor
  • CC-5013
  • LC-MS
  • Pharmacokinetics


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