Details

Autor(en) / Beteiligte

• Wang, Xin-shuai
• Sun, Jia-chun
• Yang, Rui-na
• Ren, Jing
• Liang, Shuo
• Sun, Ming
• Wang, Ying-fei
• Gao, She-Gan

Titel

Determination of cephalomannine in rat plasma by gradient elution UPLC–MS/MS method

Ist Teil von

• Journal of chromatography. B, Analytical technologies in the biomedical and life sciences, 2014-07, Vol.963, p.70-74

Ort / Verlag

Netherlands: Elsevier B.V

Erscheinungsjahr

2014

Quelle

Access via ScienceDirect (Elsevier)

Beschreibungen/Notizen

• •First report of the determination of cephalomannine in rat plasma using UPLC–MS/MS.•Sample preparation with a simple one-step protein precipitation by perchloric acid–methanol (1:9, v/v).•A relatively larger number of samples can be analyzed for 2.0min per sample. A rapid, sensitive and selective ultra-performance liquid chromatography tandem mass spectrometry (UPLC–MS/MS) was developed and validated for the determination and pharmacokinetic investigation of cephalomannine in rat plasma. Sample preparation was accomplished through a simple one-step deproteinization procedure with 0.2mL of perchloric acid–methanol (1:9, v/v) to a 0.1mL plasma sample. Plasma samples were separated by UPLC on an Acquity UPLC BEH C18 column using a mobile phase consisting of acetonitrile–0.1% formic acid in water with gradient elution. The total run time was 2.0min and the elution of cephalomannine was at 1.60min. The detection was performed on a triple quadrupole tandem mass spectrometer in the multiple reaction-monitoring (MRM) mode using the respective transitions m/z 832.8→264.1 for cephalomannine and m/z 812.6→286.0 for 10-DAT (internal standard), respectively. The calibration curve was linear over the range of 10–2000ng/mL with a lower limit of quantitation (LLOQ) of 10ng/mL. Mean recovery of cephalomannine in plasma was in the range of 80.9–85.3%. Intra-day and inter-day precision were both <11.2%. This method was successfully applied in pharmacokinetic study after intravenous administration of 5.0mg/kg cephalomannine in rats.