A method for analysis of wilfordmine in human plasma by liquid chromatography coupled with ion trap mass spectrometry.

Lixin Zhou, Hao Zhu, Xiaokun Ouyang, Jinshun Zhao, Xiaohong Chen

Index: J. Chromatogr. Sci. 53(1) , 177-82, (2014)

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Abstract

A simple and rapid liquid chromatography-ion trap mass spectrometric (LC-IT/MS) method has been developed and validated for quantification of wilfordmine in human plasma. After the protein precipitation was carried out by acetonitrile and the solution was cleaned by solid-phase extraction, the chromatographic separation was performed on a Zorbax Plus RRHD C18 column by using a mixture of acetonitrile and 10.0 mmol/L ammonium acetate solution (70:30, v/v) as the mobile phase at a flow rate of 0.7 mL/min. Detection was performed on an atmospheric-pressure chemical ionization source in the positive multiple reaction monitoring mode using aconitine as an internal standard (IS) with transitions of m/z 806→710 for wilfordmine, and 646→586 for IS, respectively. The obtained calibration curve was linear (r = 0.9992) over the concentration range of 0.5-100.0 μg/L with a lower limit of quantification of 0.5 μg/L in plasma. The intra- and interday relative standard deviations were <7.0 and 12.3%, respectively. The recoveries were between 86.0 and 97.0%. The proposed method was found to be applicable to clinical studies. © Crown copyright 2014.