Validation and implementation of a liquid chromatography/tandem mass spectrometry assay to quantitate aminoflavone (NSC 686288) in human plasma.
A reverse-phase liquid chromatography coupled to tandem mass spectrometry (LC-MS/MS) method was developed and validated for determination of aminoflavone (AF) in human plasma. Sample preparation involved a liquid-liquid extraction by the addition of 0.25 mL of plasma with 1.0 mL ethyl acetate containing 50 ng/mL of the internal standard zileuton. The analytes were separated on a Waters X-Terra MS C(18) column using a mobile phase consisting of methanol/water containing 0.45% formic acid (70:30, v/v) and isocratic flow at 0.2 mL/min for 6 min. The analytes were monitored by tandem mass spectrometry with electrospray positive ionization. Linear calibration curves were generated over the AF concentration range of 5-2000 ng/mL in human plasma. The lower limit of quantitation (LLOQ) was 5 ng/mL for AF in human plasma. The accuracy and within- and between-day precisions were within the generally accepted criteria for bioanalytical method (<15%). This method was successfully applied to characterize AF plasma concentration-time profile in the cancer patients in a phase I trial.
Wiegand
Richard
R
Karmanos Cancer Institute, Wayne State University, Detroit, MI 48201, USA.
Wu
Jianmei
J
Sha
Xianyi
X
LoRusso
Patricia
P
Heath
Elisabeth
E
Li
Jing
J
D000970:Antineoplastic Agents / Q000097:blood*; D002853:Chromatography, Liquid / Q000379:methods*; D005419:Flavonoids / Q000097:blood*; D006801:Humans; D009369:Neoplasms / Q000097:blood / Q000188:drug therapy; D053719:Tandem Mass Spectrometry / Q000379:methods*
D000970:Antineoplastic Agents; D005419:Flavonoids; C413760:aminoflavone