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Pharmacokinetic analysis of plasma bicyclol by liquid chromatography–tandem mass spectrometry
Author(s) -
Liu Mingyi,
Huang Shibo,
Wen Jinhua,
Xia Chunhua,
Zhang Hong,
Xiong Yuqing
Publication year - 2019
Publication title -
biomedical chromatography
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 0.4
H-Index - 65
eISSN - 1099-0801
pISSN - 0269-3879
DOI - 10.1002/bmc.4654
Subject(s) - chemistry , chromatography , ammonium formate , protein precipitation , pharmacokinetics , tandem mass spectrometry , mass spectrometry , extraction (chemistry) , selected reaction monitoring , detection limit , liquid chromatography–mass spectrometry , medicine
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‐CH 3 ] + ion ( m/z 373.1) subjected to demethylation as the product ion. Chromatographic separation was achieved using a Zobax Eclipse XDB‐C 18 column with a gradient elution and a mobile phase of 2 m m ammonium formate and acetonitrile. 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 >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.