Quantitative determination of helicid in rat plasma by liquid chromatography-electrospray ionization mass spectrometry and its application to preliminary pharmacokinetic studies.
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.
Jia
Yuanwei
Y
Key Laboratory of Pharmacokinetics and Drug Metabolism, China Pharmaceutical University, 1 Shennong Road, Nanjing 210038, China.
Wang
Guangji
G
Xie
Haitang
H
Dai
Xiaochang
X
Wang
Yanhua
Y
Wang
Wei
W
Xu
Meijuan
M
Wang
Rui
R
Yao
Chen
C
D000818:Animals; D001547:Benzaldehydes / Q000097:blood* / Q000493:pharmacokinetics; D002853:Chromatography, Liquid / Q000379:methods*; D051381:Rats; D017207:Rats, Sprague-Dawley; D015203:Reproducibility of Results; D021241:Spectrometry, Mass, Electrospray Ionization / Q000379:methods*
D001547:Benzaldehydes; C055677:helicide