Quantitative determination of helicid in Beagle dog plasma by liquid chromatography-electrospray ionization-mass spectrometry
JIA Yuan-wei
XIE Hai-tang
SUN Jian-guo
WANG Guang-ji
WANG Wei
YANG Hao
HUANG Qing
Abstract：Objective: To develop a sensitive and selective liquid chromatography-electrospray ionization mass spectrometry ( LC-ESI-MS) method for identification and quantification of helicid in Beagle dog plasma.Methods: The method was based on simple liquid-liquid extraction. A Luna C_(18) column ( 150mm × 2.00 mm, 3.5μm) was used as the analytical column,while a mixture of acetonitrile and 500μmol·L~(-1) ammonium chloride was used as the mobile phase. MS detection was performed using a single quadrupole mass spectrome-ter in negative selected ion monitoring (SIM) mode. The chloride adduct ions [ M + Cl]~- at m/z 319.00 and 363.05 were used to quantify helicid and bergeninum (internal standard), respectively. Results: The lower
limit of quantification of helicid was 5 ng·mL~(-1).The method was linear in the concentration range of 5～2 500 ng·mL~(-1).The intra-and inter-day precisions (RSD%) were within 10.0% for the HPLC assay.Helicid was proved to be stable during all sample storage, preparation and analytical periods. This method was successfully applied to a pharmacokinetic study in Beagle dogs after intra-gastric administration of helicid at a dose of 20 liminary pharmacokinetics studies of helicid.
Keywords：helicidbergeninumHPLC-ESI-MSpreliminary pharmacokinetics
Publication Date：2009-01-01
Online Publishing Date：2026-08-14(First online date of this platform, not the publication date of the document)
Pages：5( 2365-2369 )