Development and validation of a rapid and sensitive assay for the determination of anisodamine in 50 μL of beagle dog plasma by LC–MS/MS |
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Authors: | Wenxue Li Jun Wen Jingyu He Di Cao Fanlu Sun Jinying Li Guorong Fan |
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Institution: | 1. Department of Pharmaceutical Analysis, School of Pharmacy, Second Military Medical University, , Shanghai, P. R. China;2. College of Pharmacy, Fujian University of Traditional Chinese Medicine, , Fuzhou, Fujian, P. R. China;3. Shanghai Key Laboratory for Pharmaceutical Metabolite Research, , Shanghai, P. R. China;4. Department of Pharmacy, Guangdong Pharmaceutical University, , Guangdong, P. R. China;5. Department of Pharmacy, Xuhui Central Hospital of Shanghai, , Shanghai, P. R. China |
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Abstract: | A simple, rapid, high‐throughput, and highly sensitive LC–MS/MS was developed to determine anisodamine in a small volume (50 μL) of beagle dog plasma using atropine sulfate as the internal standard. The analyte and internal standard were isolated from 50 μL plasma samples after a one‐step protein precipitation using Sirocco 96‐well protein precipitation filtration plates. The separation was accomplished on a Hanbon Hedera CN column (100 × 4.6 mm, 5 μm) and the run time was 4 min. A Micromass Quatro Ultima mass spectrometer equipped with an ESI source was operated in the multiple reaction monitoring mode with the precursor‐to‐product ion transitions m/z 306.0→140.0 (anisodamine) and 290.0→123.9 (atropine) used for quantitation. The method was sensitive with a low LOQ of 0.05 ng/mL, and good linearity in the range 0.05–50 ng/mL for anisodamine (r2 ≥ 0.995). All the validation data, such as accuracy, intra‐ and interrun precision, were within the required limits. The method was successfully applied to the pharmacokinetic study of anisodamine hydrochloride injection in beagle dogs. |
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Keywords: | Anisodamine Dog plasma LC– MS/MS Pharmacokinetics Tropane alkaloids |
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