Research article Received: 18 August 2014,
Revised: 10 November 2014,
Accepted: 23 November 2014
Published online in Wiley Online Library: 22 January 2015
(wileyonlinelibrary.com) DOI 10.1002/bmc.3412
A rapid and sensitive LC-MS/MS method for quantification of 3,29-dibenzoyl rarounitriol in rat plasma: application to a pharmacokinetic study Chengliang Zhaoa,b†, Nan Zhangc†, Bin Chenb, Youxin Songb, Naiqiang Zhub, Long Zhaob, Changjian Liud* and Xiangwei Menga* ABSTRACT: A rapid, sensitive and high-throughput liquid chromatography–tandem mass spectrometry was established and validated to assay the concentrations of 3,29-dibenzoyl rarounitriol in rat plasma. Plasma samples were processed by liquid– liquid extraction with ethyl acetate and separated on a Hypersil Gold C18 column (50 × 4.6 mm, 3 μm) at an isocratic flow rate of 0.5 mL/min using methanol–10 mM ammonium acetate–formic acid (90:10:0.1, v/v/v) as mobile phase. The total run time was 5 min for each sample. MS/MS detection was accomplished in selected reaction monitoring mode with positive electrospray ionization. The calibration curve was linear over the concentration range of 0.125–50 ng/mL with lower limit of quantification of 0.125 ng/mL. The intra- and inter-day precisions were 0.995 for 3,29-dibenzoyl rarounitriol. The r values, slopes and intercepts were calculated using linear regression (1/x2) weighting analysis. The lowest limit of reliable quantification for the analyte was defined as the LLOQ. The intra- and inter-day precisions of analyte at LLOQ concentration were
Revised: 10 November 2014,
Accepted: 23 November 2014
Published online in Wiley Online Library: 22 January 2015
(wileyonlinelibrary.com) DOI 10.1002/bmc.3412
A rapid and sensitive LC-MS/MS method for quantification of 3,29-dibenzoyl rarounitriol in rat plasma: application to a pharmacokinetic study Chengliang Zhaoa,b†, Nan Zhangc†, Bin Chenb, Youxin Songb, Naiqiang Zhub, Long Zhaob, Changjian Liud* and Xiangwei Menga* ABSTRACT: A rapid, sensitive and high-throughput liquid chromatography–tandem mass spectrometry was established and validated to assay the concentrations of 3,29-dibenzoyl rarounitriol in rat plasma. Plasma samples were processed by liquid– liquid extraction with ethyl acetate and separated on a Hypersil Gold C18 column (50 × 4.6 mm, 3 μm) at an isocratic flow rate of 0.5 mL/min using methanol–10 mM ammonium acetate–formic acid (90:10:0.1, v/v/v) as mobile phase. The total run time was 5 min for each sample. MS/MS detection was accomplished in selected reaction monitoring mode with positive electrospray ionization. The calibration curve was linear over the concentration range of 0.125–50 ng/mL with lower limit of quantification of 0.125 ng/mL. The intra- and inter-day precisions were 0.995 for 3,29-dibenzoyl rarounitriol. The r values, slopes and intercepts were calculated using linear regression (1/x2) weighting analysis. The lowest limit of reliable quantification for the analyte was defined as the LLOQ. The intra- and inter-day precisions of analyte at LLOQ concentration were
