Mingyi Liu, Shibo Huang, Jinhua Wen
Jul 19, 2019
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Journal
Biomedical chromatography : BMC
Abstract
Bicyclol is a synthetic drug widely used to treat chronic hepatitis B. This study aimed to develop a selective, sensitive, and high-throughput liquid chromatography-tandem mass spectrometric method for the detection of bicyclol in human plasma. Bicyclol was detected using a multiple-reaction monitoring mode, with ammonium-adduct ions (m/z 408.2) as the precursor ion and the [M-CH3 ]+ ion (m/z 373.1) subjected to demethylation as the product ion. Chromatographic separation was achieved using a Zobax Eclipse XDB-C18 column with a gradient elution and a mobile phase of 2-mM ammonium formate and methanol. Bicyclol was extracted from plasma matrix by precipitation. A linear-detection response was obtained for bicyclol ranging from 0.500 to 240 ng/mL, and the lower limit of quantification was 0.500 ng/mL. The intra- and inter-day precisions were all ≤7.4%, and the accuracies were within ± 6.0%. The extraction recovery was over 95.9%, and the matrix effects were between 96.0% and 108%. Bicyclol was found to be unstable in human plasma at room temperature, but the degradation was minimized by conducting sample collection and preparation in an ice bath. The validated method was successfully applied to investigate the pharmacokinetics of bicyclol tablets in six healthy Chinese volunteers.