title: Determination of palmatine in canine plasma by liquid chromatography-tandem mass spectrometry with solid-phase extraction.
abstract: A sensitive and specific high-performance liquid chromatography-tandem mass spectrometry (HPLC-MS-MS) method has been developed and validated for the determination of palmatine in canine plasma. Palmatine and jatrorrhizine (internal standard, I.S.) were extracted from plasma samples by solid-phase extraction (SPE) using Oasis HLB cartridges. The chromatographic separation was performed on a Waters XTerra MS C(18) reversed-phase column at 30 degrees C. The gradient mobile phase, delivered at 0.25 mL/min, was composed of a mixture of acetonitrile -0.1% (v/v) acetic acid aqueous solution adjusted to pH 2.8 with triethylamine. Positive electrospray ionization was utilized as the ionization source. Palmatine and the internal standard (I.S.) were determined using multiple reaction monitoring (MRM) of precursor-->product ion transitions at m/z 352-->336 and m/z 338-->322, respectively. The lower limit of quantification (LLOQ) was 0.1 ng/mL using 100 microL plasma samples and the linear calibration range was from 0.1 to 500 ng/mL. The inter-day and intra-day RSDs were lower than 9.9% and the recoveries of palmatine ranged from 87.3 to 100.9%. The mean extraction recoveries of palmatine and the I.S. were 99.2 and 96.8%, respectively. The method has been successfully applied to the pharmacokinetic studies of palmatine in beagle dogs after oral administration and intramuscular injection of palmatine.
authors.affiliation: Department of Pharmacognosy, School of Pharmacy, Fudan University, Shanghai 200032, PR China.
authors.forename: Jian-ming
authors.initials: JM
authors.lastname: Huang
authors.forename: Guo-quan
authors.initials: GQ
authors.lastname: Wang
authors.forename: Yu-e
authors.initials: YE
authors.lastname: Jin
authors.forename: Teng
authors.initials: T
authors.lastname: Shen
authors.forename: Weiyu
authors.initials: W
authors.lastname: Weng
mesh_terms: D000818:Animals; D001600:Berberine Alkaloids / Q000097:blood* / Q000493:pharmacokinetics; D002851:Chromatography, High Pressure Liquid / Q000379:methods*; D004285:Dogs; D008297:Male; D012680:Sensitivity and Specificity; D053719:Tandem Mass Spectrometry / Q000379:methods*
chemical_list: D001600:Berberine Alkaloids; C005413:palmatine