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Quantitation and pharmacokinetics of 1,4-diamino-2,3-dicyano-1,4-bis (2-aminophenylthio) butadiene (U0126) in rat plasma by liquid chromatography-tandem mass spectrometry

Authors
 신상준 ; 황지원 
Citation
 Journal of Separation Science, Vol.36(2) : 239~245, 2013 
Journal Title
 Journal of Separation Science 
ISSN
 1615-9306 
Issue Date
2013
Abstract
A simple, robust, and rapid LC-MS/MS method was developed for the quantitation of U0126 and validated in rat plasma. Plasma samples (20 μL) were deproteinized using 200 μL ACN containing 30 ng/mL of chlorpropamide, internal standard. Chromatographic separation performed on an Agilent Poroshell 120 EC-C(18) column (4.6 × 50 mm, 2.7 μm particle size) with an isocratic mobile phase consisting of a 70:30 v/v mixture of ACN and 0.1% aqueous formic acid. Each sample was run at 0.6 mL/min for a total run time of 2 min per sample. Detection and quantification were performed using a mass spectrometer in selected reaction-monitoring mode with positive ESI at m/z 381 → 123.9 for U0126 and m/z 277 → 175 for the internal standard. The standard curve was linear over a concentration range of 20-5000 ng/mL with correlation coefficients greater than 0.9965. Precision, both intra- and interday, was less than 10.1% with an accuracy of 90.7-99.4%. No matrix effects were observed. U0126 in rat plasma degraded approximately 41.3% after 3-h storage at room temperature. To prevent degradation, sample handling should be on an ice bath and all solutions kept at 4°C. This method was successfully applied to a pharmacokinetic study of U0126 at various doses in rats
URI
http://ir.ymlib.yonsei.ac.kr/handle/22282913/88028
DOI
10.1002/jssc.201200779
Appears in Collections:
1. 연구논문 > 1. College of Medicine > Medical Research Center
1. 연구논문 > 1. College of Medicine > Dept. of Internal Medicine
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Link
 http://dx.doi.org/10.1002/jssc.201200779
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