Section 51
Chapter 50,091

Quantitative determination of helicid in rat plasma by liquid chromatography-electrospray ionization mass spectrometry and its application to preliminary pharmacokinetic studies

Jia, Y.; Wang, G.; Xie, H.; Dai, X.; Wang, Y.; Wang, W.; Xu, M.; Wang, R.; Yao, C.

Journal of Chromatography. B Analytical Technologies in the Biomedical and Life Sciences 847(2): 72-77


ISSN/ISBN: 1570-0232
PMID: 17046341
DOI: 10.1016/j.jchromb.2006.09.020
Accession: 050090237

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A sensitive and selective liquid chromatography-electrospray ionization mass spectrometry (LC-ESI-MS) method was developed for the identification and quantification of helicid in rat plasma. The method was based on simple liquid-liquid extraction (LLE). A Kromasil C18 column (150mmx2.00mm, 3.5microm) was used as the analytical column, while a mixture of acetonitrile and 500microM ammonium chloride was used as the mobile phase. MS detection was performed using a single quadrupole mass spectrometer in a negative selected ion monitoring (SIM) mode. The deprotonated molecules [M+Cl](-) at m/z 319.00 and 363.05 were used to quantify helicid and bergeninum (internal standard, I.S.), respectively. The lower limit of quantification of helicid was 1ng/ml. The method was linear in the concentration range of 1-1000ng/ml. The intra-day and inter-day precisions (R.S.D.%) were within 10.0% for the analyte. Helicid proved to be stable during all sample storage, preparation and analytical periods. The method was successfully applied to a pharmacokinetic study in rats after intragastric administration of helicid with a dose of 50mg/kg. Only 50microl of rat plasma at each sampling time was needed for analysis. The proposed method enables unambiguous identification and quantification for the preliminary pharmacokinetic studies of helicid.

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