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Development and validation of an LC‐MS/MS method for the determination of bullatine A in rat plasma: application to a pharmacokinetic study
Author(s) -
Teng ShiYong,
Zhang SiXi,
Niu Kai,
Zhai LiJie,
Wang ShiJi
Publication year - 2015
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.3498
Subject(s) - chemistry , chromatography , formic acid , selected reaction monitoring , protein precipitation , triple quadrupole mass spectrometer , acetonitrile , pharmacokinetics , mass spectrometry , detection limit , tandem mass spectrometry , analytical chemistry (journal) , pharmacology , medicine
Abstract Bullatine A is a diterpenoid alkaloid of Xue‐Shang‐Yi‐Zhi‐Hao ( Aconitum brachypodum ), which is widely used in traditional Chinese medicine for the treatment of rheumatism and pain. The plasma levels of bullatine A were measured by a rapid and sensitive LC‐MS/MS method. Samples were prepared using acetonitrile precipitation and the separation of bullatine A was achieved on a Capcell Pak MG‐C 18 column by isocratic elution using acetonitrile (phase A) and 0.1% formic acid (phase B, pH 4.0; A:B, 30:70, v/v) as the mobile phase at a flow rate of 0.5 mL/min. Detection was performed on a triple‐quadrupole tandem mass spectrometer by multiple‐reaction monitoring of the transitions at m / z 344.2 → 105.2 for bullatine A and m / z 256.2 → 167.1 for the internal standard. The linearity was found to be within the concentration range of 1.32–440 ng/mL with a lower limit of quantification of 1.32 ng/mL. Only 1.3 min was needed for an each analytical run. This method was successfully applied in the determination of the active component bullatine A in rat plasma after intramuscular administration of A . brachypodum injection. Copyright © 2015 John Wiley & Sons, Ltd.