科研之友
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摘要
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 C-18 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 mu g/L with a lower limit of quantification of 0.5 mu g/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.
