title: A rapid and sensitive LC-MS/MS method for the determination of linarin in small-volume rat plasma and tissue samples and its application to pharmacokinetic and tissue distribution study.
abstract: A rapid and sensitive LC-MS/MS method was developed for the determination of linarin in small-volume rat plasma and tissue sample. Sample preparation was employed by the combination of protein precipitation (PPT) and liquid-liquid extraction (LLE) to allow measurement over a 5-order-of-magnitude concentration range. Fast chromatographic separation was achieved on a Hypersil Gold column (100 × 2.1 mm i.d., 5 µm). Mass spectrometric detection was achieved using a triple-quadrupole mass spectrometer equipped with an electrospray ionization interface operating in positive ionization mode. Quantification was performed using selected reaction monitoring of precursor-product ion transitions at m/z 593 → 285 for linarin and m/z 447 → 271 for baicalin (internal standard). The total run time was only 2.8 min per sample. The calibration curves were linear over the concentration range of 0.4-200 µg/mL for PPT and 0.001-1.0 µg/mL for LLE. A lower limit of quantification of 1.0 ng/mL was achieved using only 20 μL of plasma or tissue homogenate. The intra- and inter-day precisions in all samples were ≤14.7%, while the accuracy was within ±5.2% of nominal values. The validated method has been successfully applied to pharmacokinetic and tissue distribution study of linarin.
authors.affiliation: Laboratory of Drug Metabolism and Pharmacokinetics, School of Pharmacy, Shenyang Pharmaceutical University, Shenyang, 110016, People's Republic of China.|School of Chinese Materia Medica, Tianjin University of Traditional Chinese Medicine, Tianjin, 300193, People's Republic of China.
authors.forename: Xinchi
authors.initials: X
authors.lastname: Feng
authors.affiliation: Laboratory of Drug Metabolism and Pharmacokinetics, School of Pharmacy, Shenyang Pharmaceutical University, Shenyang, 110016, People's Republic of China.
authors.forename: Youping
authors.initials: Y
authors.lastname: Liu
authors.affiliation: Laboratory of Drug Metabolism and Pharmacokinetics, School of Pharmacy, Shenyang Pharmaceutical University, Shenyang, 110016, People's Republic of China.
authors.forename: Xin
authors.initials: X
authors.lastname: Wang
authors.affiliation: Laboratory of Drug Metabolism and Pharmacokinetics, School of Pharmacy, Shenyang Pharmaceutical University, Shenyang, 110016, People's Republic of China.
authors.forename: Xin
authors.initials: X
authors.lastname: Di
mesh_terms: D000818:Animals; D002851:Chromatography, High Pressure Liquid / Q000191:economics / Q000379:methods*; D031180:Cirsium / Q000737:chemistry; D006027:Glycosides / Q000097:blood / Q000302:isolation & purification / Q000493:pharmacokinetics*; D057230:Limit of Detection; D059625:Liquid-Liquid Extraction / Q000191:economics / Q000379:methods; D008297:Male; D051381:Rats; D017207:Rats, Sprague-Dawley; D053719:Tandem Mass Spectrometry / Q000191:economics / Q000379:methods*; D014018:Tissue Distribution
chemical_list: D006027:Glycosides; C008282:linarin
keywords: LC-MS/MS; linarin; pharmacokinetics; rats; tissue distribution