A sensitive and specific LC-MS/MS method employing positive electrospray ionization for the determination of ARQ 501 (beta-lapachone) in (nu/nu) mouse plasma and tumor tissue is described. Samples were processed using protein precipitation with acetonitrile. A d6 analog of ARQ 501 was used as the internal standard (IS). The analytes were separated using a Zorbax SB8 column (30 mm x 2.1 mm i.d. 5 microm particle size) and analyzed in the multiple reaction monitoring (MRM) mode using mass transitions of 243>159 and 249>159 m/z for ARQ 501 and d6-ARQ 501, respectively. The lower limit of quantitation (LLOQ) for ARQ 501 was 3.0 ng/mL. The calibration curve was linear in the range of 3.0-2000 ng/mL with a correlation coefficient better than 0.99. Intra- and inter-batch precisions were within 8.4
作者:R E, Savage;T, Hall;K, Bresciano;J, Bailey;M, Starace;T C K, Chan
来源:Journal of chromatography. B, Analytical technologies in the biomedical and life sciences 2008 年 872卷 1-2期