Journal
JOURNAL OF CHROMATOGRAPHY B-ANALYTICAL TECHNOLOGIES IN THE BIOMEDICAL AND LIFE SCIENCES
Volume 878, Issue 25, Pages 2348-2352Publisher
ELSEVIER SCIENCE BV
DOI: 10.1016/j.jchromb.2010.07.019
Keywords
MK-0752; Online sample preparation; High turbulence liquid chromatography (HTLC); Electrospray tandem mass spectrometry (ESI-MS/MS)
Funding
- NCI NIH HHS [P30 CA021765, P01 CA 23099, P01 CA023099, CA 21765, U01 CA081457, P30 CA021765-32, P01 CA023099-239005] Funding Source: Medline
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A sensitive and rapid HTLC-ESI-MS/MS method with an advanced online sample preparation was developed for determination of the gamma-secretase inhibitor MK-0752 in human plasma using an internal standard. Plasma samples (100 mu l) were diluted and injected directly onto an online extraction column (Cohesive Cyclone MAX 0.5 mm x 50 mm, >30 mu m), the sample matrix was washed out with an aqueous solution, and retained analytes were eluted out and transferred directly to the analytical column (Phenomenex Gemini 3 mu. C18 110A, 50 mm x 2.0 mm at 50 degrees C) for separation using a gradient mobile phase. The eluted analytes were then detected on an API-3000 LC-MS/MS System with ESI and a negative multiple reaction monitoring mode. The monitored ion transitions were m/z 441 -> 175 for MK-0752 and 496 175 for the internal standard. Online extraction recoveries were 81%. The method was validated and was linear in the range of 0.05-50 mu g/mL.. Within-day and between-day precisions were <8.6%, and accuracies were 0.7 and 7.1%. This method was applied to the measurement of plasma MK-0752 levels in a Phase I study of pediatric patients with recurrent or refractory brain tumors. (C) 2010 Elsevier B.V. All rights reserved.
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