title: Validated liquid chromatography-tandem mass spectrometry method for quantitative determination of dauricine in human plasma and its application to pharmacokinetic study.
abstract: A highly sensitive and selective LC-MS/MS method was developed and validated for the determination of dauricine in human plasma, using protopine as internal standard (IS). The analyte and IS were extracted by liquid-liquid extraction and analyzed by LC-MS/MS. Chromatographic separation was performed on Agilent TC-C(18) column with a mobile phase of methanol-water-glacial acetic acid (60:40:0.8, v/v/v) at a flow rate of 0.7 mL/min. Detection was performed on a triple quadrupole tandem mass spectrum by multiple reaction monitoring (MRM) mode using the electrospray ionization technique in positive mode. The method was linear over the concentration range of 1-200 ng/mL. The lower limit of quantification (LLOQ) was 1 ng/mL in human plasma with acceptable precision and accuracy. The intra- and inter-day precision was less than 5.9% determined from quality control (QC) samples at concentrations of 2.0, 20.0 and 160 ng/mL, and the accuracy was within +/-9.9%. This method was successfully applied for the evaluation of pharmacokinetics of dauricine after oral doses of 100, 300 and 600 mg phenolic alkaloids of menispermum dauricum tablet (PAMDT) to 12 Chinese healthy volunteers.
authors.affiliation: School of Pharmacy, Shenyang Pharmaceutical University, 103 Wenhua Road, Shenyang 110016, PR China.
authors.forename: Xiaoying
authors.initials: X
authors.lastname: Liu
authors.forename: Qian
authors.initials: Q
authors.lastname: Liu
authors.forename: Dongmei
authors.initials: D
authors.lastname: Wang
authors.forename: Xueya
authors.initials: X
authors.lastname: Wang
authors.forename: Peng
authors.initials: P
authors.lastname: Zhang
authors.forename: Haiyan
authors.initials: H
authors.lastname: Xu
authors.forename: Hui
authors.initials: H
authors.lastname: Zhao
authors.forename: Huaiqing
authors.initials: H
authors.lastname: Zhao
mesh_terms: D053119:Benzophenanthridines / Q000032:analysis; D044182:Benzylisoquinolines / Q000097:blood* / Q000737:chemistry / Q000493:pharmacokinetics; D001600:Berberine Alkaloids / Q000032:analysis; D002853:Chromatography, Liquid / Q000379:methods*; D004355:Drug Stability; D006801:Humans; D016018:Least-Squares Analysis; D008297:Male; D015203:Reproducibility of Results; D012680:Sensitivity and Specificity; D053719:Tandem Mass Spectrometry / Q000379:methods*; D044005:Tetrahydroisoquinolines / Q000097:blood* / Q000737:chemistry / Q000493:pharmacokinetics
chemical_list: D053119:Benzophenanthridines; D044182:Benzylisoquinolines; D001600:Berberine Alkaloids; D044005:Tetrahydroisoquinolines; C035934:dauricine; C009093:protopine