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Determination and stability of CP-31398 in plasma from experimental animals by LC-MS/MS
- Source :
-
Journal of Pharmaceutical & Biomedical Analysis . Dec2011, Vol. 56 Issue 4, p809-814. 6p. - Publication Year :
- 2011
-
Abstract
- Abstract: A sensitive and accurate approach for the determination of CP-31398 (N-{2-[(E)-2-(4-methoxy-phenyl)-vinyl]-quinazolin-4-yl}-N′,N′-dimethyl-propane-1,3-diamine hydrochloride) in rat and dog plasma by LC-MS/MS was validated to support preclinical toxicological and pharmacological studies. Based on the results of stability experiments with diluted CP-31398 solutions using NMR, LC-MS/MS and LC-Q-TOF, all sample preparation and handling steps were performed under yellow light to avoid CP-31398 decomposition. CP-31398 was extracted by protein precipitation with acetonitrile and separated using a Phenomenex Luna 3μm phenyl-hexyl, 100Å, 30×2.0mm column (rat plasma) or a Phenomenex Synergi 4μ Polar-RP, 80Å, 30×2.0mm column (dog plasma) at a flow rate of 0.30mL/min. The mobile phase consisted of A: 1% formic acid in water and B: 1% formic acid in methanol or acetonitrile. Total run times for rat and dog samples were 7 and 8min, respectively, with accompanying retention times of 1.8 for both columns. A turbo ion spray interface was used as the ion source operating in positive mode. Calibration curves were linear from 5 to 1000ng/mL. Linearity was assessed using the external standard method. Within-run and between-run accuracy was 93–109% of the true value for all analytes with precision (SD) of 8% or less for all experiments. The validated method was applied to preclinical toxicology studies in rats and dogs after oral administration of CP-31398. [Copyright &y& Elsevier]
Details
- Language :
- English
- ISSN :
- 07317085
- Volume :
- 56
- Issue :
- 4
- Database :
- Academic Search Index
- Journal :
- Journal of Pharmaceutical & Biomedical Analysis
- Publication Type :
- Academic Journal
- Accession number :
- 64482773
- Full Text :
- https://doi.org/10.1016/j.jpba.2011.07.013