title: Simultaneous determination of three bufadienolides in rat plasma after intravenous administration of bufadienolides extract by ultra performance liquid chromatography electrospray ionization tandem mass spectrometry.
abstract: A novel, rapid and specific ultra performance liquid chromatography electrospray ionization tandem mass spectrometry (UPLC-ESI-MS/MS) method has been developed for simultaneous determination and pharmacokinetic studies of three bufadienolides (bufalin, cinobufagin and resibufogenin) in rat plasma. The analytes, bufalin, cinobufagin, resibufogenin and the internal standard, diphenhydramine were extracted from rat plasma samples by a one-step liquid-liquid extraction and separated on an ACQUITY UPLCtrade mark BEH C(18) column with gradient elution using a mobile phase composed of acetonitrile and water (containing 0.1% formic acid) at a flow rate of 0.20 mL min(-1). Detection was carried out on a triple-quadrupole tandem mass spectrometer in the multiple reaction monitoring (MRM) mode via an electrospray ionization (ESI) interface. The three bufadienolides could be simultaneously determined within 3.0 min. Linear calibration curves were obtained over the concentration ranges of 1.0-200 ng mL(-1) for all the analytes. The intra- and inter-day precisions (relative standard deviation (R.S.D.)) were less than 11.35 and 10.87%, respectively. The developed method was applied for the first time to the pharmacokinetic studies of bufadienolides in rats following a single intravenous administration of 2.10 mg kg(-1) bufadienolides.
authors.affiliation: Department of Pharmaceutics, Shenyang Pharmaceutical University, 103 Wenhua Road, Shenyang 110016, PR China.
authors.forename: Yu
authors.initials: Y
authors.lastname: Zhang
authors.forename: Xing
authors.initials: X
authors.lastname: Tang
authors.forename: Xiaoliang
authors.initials: X
authors.lastname: Liu
authors.forename: Fang
authors.initials: F
authors.lastname: Li
authors.forename: Xia
authors.initials: X
authors.lastname: Lin
mesh_terms: D000818:Animals; D002018:Bufanolides / Q000008:administration & dosage / Q000097:blood* / Q000493:pharmacokinetics; D002138:Calibration; D002851:Chromatography, High Pressure Liquid / Q000379:methods*; D007262:Infusions, Intravenous; D008297:Male; D051381:Rats; D017208:Rats, Wistar; D012015:Reference Standards; D015203:Reproducibility of Results; D012680:Sensitivity and Specificity; D021241:Spectrometry, Mass, Electrospray Ionization / Q000379:methods*; D053719:Tandem Mass Spectrometry / Q000379:methods*
chemical_list: D002018:Bufanolides