Determination of tubuloside B by LC‐MS/MS and its application to a pharmacokinetic study in rats |
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Authors: | Shenbao Yang Ruiying Qu Peilu Sun Shan Xiong Siyi Yan Zhipeng Deng |
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Institution: | 1. Jiaozhou People's Hospital, Qingdao, China;2. Shandong Academy of Medical Sciences, Institute of Materia Medica, Jinan, China;3. Key Laboratory for Biotech‐Drugs Ministry of Health, Jinan, China;4. Key Laboratory for Rare and Uncommon Diseases of Shandong Province, Jinan, China;5. Department of Anesthesiology, Beijing Tsinghua Changgung Hospital, Beijing, China;6. Zhipeng Deng, Institute of Materia Medica, Shandong Academy of Medical Sciences, Jinan, China. |
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Abstract: | Tubuloside B, a novel neuroprotective phenylethanoid, is a major active constituent of Cistanche tubulosa and Cistanche deserticola. A specific and sensitive liquid chromatography tandem mass spectrometry (LC‐MS/MS) method has been developed and validated for the quantification of tubuloside B in rat plasma. Sample preparation was conducted through a protein‐precipitation extraction with methanol using tubuloside A as internal standard (IS). Chromatographic separation was achieved using a Capcell Pak C18 column (2.0 × 50 mm, 5 μm) with a mobile phase of methanol–10 mm ammonium acetate buffer (70:30, v/v) in an isocratic elution. Mass spectrometry analysis was performed in negative ionization mode with selected reaction monitoring transitions at m/z 665.1 → 160.9 for tubuloside B, and m/z 827.1 → 160.9 for IS. Calibration curves were linear over the range of 1.64–1640 ng/mL for plasma samples samples (R2 > 0.990). The lower limit of quantification (LLOQ) was 1.64 ng/mL. The intra‐ and inter‐day accuracy was between 92.3 and 113.0% with the RSD <9.23% at all LLOQ and quality control levels. Finally, this method was successfully applied in the pharmacokinetics study of tubuloside B after intravenous administration. |
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Keywords: | tubuloside B liquid chromatography– tandem mass spectrometry pharmacokinetic study |
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