A specific, sensitive and robust LC–MS/MS method was developed and validated for the quantification of deoxyelephantopin in rat plasma using simvastatin as an internal standard as per regulatory guidelines of Bioanalytical Method Validation. Plasma sample was prepared through liquid-liquid extraction. Chromatographic separation was performed on an Agela-C18 analytical column (1.8 μm, 2.1 mm × 50 mm) with an isocratic mobile phase consisting of 0.05% formic acid (dissolved in acetonitrile) and water (55:45, v/v) at a flow rate of 0.5 ml/min. The column oven was maintained at 40 °C and the injection volume was 4 μl. Elution of deoxyelephantopin and the internal standard occurred at 5.1 and 6.3 min, respectively. The total chromatographic run time was 7.5 min. A linear response function was constructed in the concentration range of 13.2–2640 ng/ml. The intra- and inter-day precision and accuracy were in the range of 1.4–14.8% and –11.7 to 14.1%, respectively. The validated LC–MS/MS was successfully applied to the pharmacokinetic study of deoxyelephantopin after intravenous injection of 1, 2 and 4 mg/kg and oral administration of 7.5, 15 and 30 mg/kg deoxyelephantopin in rats. After oral and intravenous administration, the Cmax and AUC values of deoxyelephantopin increased dose-dependently.

/pdf/lc-ms-ms-determination-of-deoxyelephantopin-a-novel-anti-28a0jehf7z.pdf

LC–MS/MS determination of deoxyelephantopin, a novel anti-tumor candidate in rat plasma and its application to a pharmacokinetic study in rats

Objective To establish qualitative and quantitative methods for the quality evaluation of deoxyelephantopin in Elephantopus scaber L. Methods Qualitative analysis was performed on the thin-layer per- coated TLC-plates silia gel G,with petroleum ether( 60 ~90℃)-ethyl acetate( 2∶3),after spraying with 10% vanillin sulfuric acid solution,heated at 105℃ until the spots were clear.Quantitative analysis was performed on Kromasil C18( 250 mm ×4.6 mm,5 μm). The mobile phase was acetonitrile-water( 35∶65) at the flow rate of 1. 0 mL·min- 1,the detection wavelength was 208 nm,and the column temperature was 30℃. Results Test products had the same color blotches on relative location of chromatography with Chinese herbal medicine. Deoxyelephantopin showed good linear regression( r = 1. 000) within test ranges of 0. 005 915 ~ 0. 059 15 g·L- 1. The average recovery( n = 6) was 98. 75%,and the range of contents in the samples were 0. 072% ~ 0. 15%. Conclusions The methods developed are sensitive,reliable and useful for the analysis of samples purchased from different areas and can be used for the quality control of Elephantopus scaber L.

Qualitative and quantitative analysis of deoxyelephantopin in Elephantopus scaber L.

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Qualitative and quantitative analysis of deoxyelephantopin in Elephantopus scaber L.