Abstract
A rapid and sensitive method for the quantitative determination of picroside II in rat plasma was developed and validated using liquid chromatographic separation with tandem mass spectrometric detection. The analytes of interest were extracted from rat plasma samples by ethyl acetate after acidification with 1.0% acetic acid solution. Chromatographic separation was achieved on a Hypersil GOLD column (50 × 2.1 mm I.D., 5 μm) using a mobile phase consisting of acetonitrile–0.1% formic acid solution (30:70, v/v) at a flow rate of 0.2 mL min−1. Detection was performed on a triple quadrupole tandem mass spectrometer by selected reaction monitoring (SRM) mode via electrospray ionization (ESI). The calibration curve was linear in the concentration range of 1.00–400 ng mL−1 in rat plasma, with a 1.00 ng mL−1 lower limit of quantification (LLOQ). Satisfactory results were achieved for intraday repeatability [relative standard deviation (RSD) = 6.4–12.4%] and inter-day precision (RSD = 6.8–14.7%). The accuracy in terms of relative error ranged from −2.1 to 10.0%. The extraction recoveries of picroside II and icariin (internal standard) were 80.0 and 89.3%, respectively. The developed method was successfully employed to determine picroside II plasma concentrations after oral administration to Wistar rats.
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Acknowledgments
This work was supported by the National Natural Science Foundation of the People’s Republic of China (No. 30371643, 30572183), the New Century Excellent Talents in University (NCET), Research Fund for the Doctoral Program of Higher Education of China, Foundation of Beijing Educational Committee (No. KZ200610025013), and Scientific Research Foundation for Returned Scholars, Ministry of Education of China awarded to J. He, the New Star Plan of Science & Technology of Beijing of China (No. 2007B065) and Basic and clinical research foundation of Capital Medical University (No. 2007JL01).
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Ma, Y., Cheng, S., Leski, M.L. et al. Development and Validation of a Sensitive LC–Tandem-MS Method for the Quantitative Determination of Picroside II in Rat Plasma. Chroma 68, 1027–1032 (2008). https://doi.org/10.1365/s10337-008-0809-x
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DOI: https://doi.org/10.1365/s10337-008-0809-x