Abstract
Wilforidine is a potentially efficient medicine to cure autoimmune diseases. In this paper, a sensitive and selective liquid chromatographic method coupled with atmospheric -pressure chemical ionization mass spectrometry (LC–APCI–MS/MS) has been developed for quantification of wilforidine in human plasma. Samples were deproteinized with acetonitrile and cleaned by solid-phase extraction. The chromatographic separation was performed on an analytical RRHD C18 column (50 × 2.1 mm) using ammonium acetate solution (10.0 mmol L−1)/acetonitrile (30/70, v/v) as the mobile phase at a flow rate of 0.7 mL min−1. Detection was carried out by the positive multiple reaction monitoring mode with transitions of m/z 780 → 684 for wilforidine, and 646 → 586 for aconitine (internal standard), respectively. The calibration curve was linear (r = 0.9991) in the concentration range of 0.5–100.0 μg L−1 with a lower limit of quantification of 0.5 μg L−1 in plasma. Intra- and inter-day relative standard deviations were less than 6.8 and 13.1 %, respectively, and the recoveries were between 88.0 and 96.0 %. This accurate and highly specific assay provides a useful method for evaluating the pharmacokinetics of wilforidine in human plasma.
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Acknowledgments
This research was supported by Zhejiang Provincial nonprofit technology research program of China (No. 2013C31140), Ningbo Natural Science Foundation in Zhejiang (2011A610058) and Zhejiang Provincial Program for the Cultivation of High-level Innovative Health Talents.
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Cai, M., Shen, C. & Jin, M. Sensitive Analysis of Wilforidine in Human Plasma by LC-APCI-MS/MS. Chromatographia 76, 985–991 (2013). https://doi.org/10.1007/s10337-013-2504-9
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DOI: https://doi.org/10.1007/s10337-013-2504-9