title: Quantitative determination of helicid in rat biosamples by liquid chromatography electrospray ionization mass spectrometry.
abstract: A simple liquid chromatography electrospray ionization mass spectrometry (LC-ESI-MS) method with highly improved sensitivities for the determination of helicid in rat bile, urine, feces and most tissues was developed. The tissues and feces were firstly homogenized mechanically using deionized water as the media. Bile, urine, tissues and feces homogenates were extracted by liquid-liquid extraction with n-butyl alcohol for sample preparation. The subsequent analysis procedures were performed on a Shimadzu LCMS2010A system (electrospray ionization single quadrupole mass analyzer). A Luna C(18) column (150 mm x 2.00 mm, 5 microm) was used as the analytical column, while a mixture of acetonitrile and ammonium chloride water solution was used as the mobile phase. The proportions of mobile phase were changed timely according to gradient programs. Chlorinated adducts of molecular ions [M+Cl](-) at m/z 319.00 and 363.05 were used to quantify helicid and bergeninum (internal standard), respectively. The method was validated to be accurate, precise and rugged with good linearity. The proposed method was successfully applied to the preclinical tissue distribution and excretion studies of helicid in rats.
authors.affiliation: Key Laboratory of Pharmacokinetics and Drug Metabolism, China Pharmaceutical University, 24# Tongjia Xiang Street, Nanjing 210009, China.
authors.forename: Yuanwei
authors.initials: Y
authors.lastname: Jia
authors.forename: Haitang
authors.initials: H
authors.lastname: Xie
authors.forename: Guangji
authors.initials: G
authors.lastname: Wang
authors.forename: Jianguo
authors.initials: J
authors.lastname: Sun
authors.forename: Wei
authors.initials: W
authors.lastname: Wang
authors.forename: Huang
authors.initials: H
authors.lastname: Qing
authors.forename: Xuan
authors.initials: X
authors.lastname: Wang
authors.forename: Hao
authors.initials: H
authors.lastname: Yang
authors.forename: Meijuan
authors.initials: M
authors.lastname: Xu
authors.forename: Yi
authors.initials: Y
authors.lastname: Gu
authors.forename: Chen
authors.initials: C
authors.lastname: Yao
authors.forename: Jie
authors.initials: J
authors.lastname: Shen
mesh_terms: D000818:Animals; D001547:Benzaldehydes / Q000008:administration & dosage / Q000032:analysis* / Q000493:pharmacokinetics / Q000652:urine; D001646:Bile / Q000737:chemistry*; D002851:Chromatography, High Pressure Liquid / Q000379:methods*; D005243:Feces / Q000737:chemistry; D005260:Female; D008297:Male; D051381:Rats; D021241:Spectrometry, Mass, Electrospray Ionization / Q000379:methods*; D014018:Tissue Distribution
chemical_list: D001547:Benzaldehydes; C055677:helicide