《Determination and pharmacokinetics of DT-13 in rat plasma by LC–MS》.pdf

Journal of Pharmaceutical and Biomedical Analysis 56 (2011) 650–654 Contents lists available at ScienceDirect Journal of Pharmaceutical and Biomedical Analysis j o u r na l h o me p a g e : w w w. elsev /locate/jpba Short communication Determination and pharmacokinetics of DT-13 in rat plasma by LC–MS Lin-lin Chen 1, Wei-wei Yuan 1, Zheng-fang Hu, Jin Qi, Dan-ni Zhu, Bo-yang Yu ∗ Department of Complex Prescription of Traditional Chinese Medicine, China Pharmaceutical University, Nanjing 211198, China a r t i c l e i n f o a b s t r a c t Article history: A sensitive and specific LC–MS assay for DT-13 in rat plasma was developed. DT-13 is an active steroidal Received 27 January 2011 saponin present in Liriopes Radix and is developed as an anti-tumor drug candidate. The samples were Received in revised form 1 July 2011 extracted by acetonitrile-mediated plasma protein precipitation. The chromatographic separation was Accepted 4 July 2011 carried out using a Ultimate C18 column (250 mm ×4.6 mm, i.d., 5 m) with a mobile phase composed Available online 12 July 2011 of acetonitrile: 5 mmol/L aqueous ammonium acetate (60:40, v:v). The method was validated and the specificity, linearity (r2 = 0.9980 within 10–1000 ng/mL), lower limit of quantitation (LLOQ, 10 ng/mL), Keywords: precision (intra- and inter-day <12.3%), accuracy (93.4–106.3%), recovery (91.0 ± 4.7%) and stability were DT-13 determined. The method