Quantitative determination of the HIV protease inhibitor atazanavir (BMS-232632) in human plasma by liquid chromatography-tandem mass spectrometry following automated solid-phase extraction.
A selective, accurate, and reproducible LC-MS-MS assay was developed for the determination of the HIV protease inhibitor atazanavir (BMS-232632) in human plasma samples. The method involved automated solid-phase extraction of atazanavir and a stable isotope analog internal standard (I.S.) using Oasis HLB 10 mg 96-well SPE plates. A portion of the reconstituted sample residue was injected onto a C(18) HDO analytical column which was configured with a triple quad mass spectrometer for analyte determination by positive ion electrospray. The assay was linear from 1.00 to 1,000 ng/ml with a lower limit of quantitation of 1.00 ng/ml. The inter- and intra-day coefficients of variation (C.V.) for the assay were <4%, and the accuracy was 99-102%. Atazanavir was stable in human plasma for at least 109 h at room temperature and for at least 1 year at -20 degrees C.
Schuster
A
A
Drug Disposition and Bioanalytical Sciences, Bristol-Myers Squibb Pharmaceutical Research Institute, One Squibb Drive, New Brunswick, NJ 08903, USA.
Burzawa
S
S
Jemal
M
M
Loizillon
E
E
Couerbe
P
P
Whigan
D
D
D000069446:Atazanavir Sulfate; D001331:Automation; D002138:Calibration; D002851:Chromatography, High Pressure Liquid / Q000379:methods*; D017320:HIV Protease Inhibitors / Q000097:blood*; D006801:Humans; D013058:Mass Spectrometry / Q000379:methods*; D009842:Oligopeptides / Q000097:blood*; D011725:Pyridines / Q000097:blood*; D012015:Reference Standards; D012680:Sensitivity and Specificity
D017320:HIV Protease Inhibitors; D009842:Oligopeptides; D011725:Pyridines; D000069446:Atazanavir Sulfate