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Quantitation and pharmacokinetics of 1,4‐diamino‐2,3‐dicyano‐1,4‐bis (2‐aminophenylthio) butadiene ( U 0126) in rat plasma by liquid chromatography‐tandem mass spectrometry
Author(s) -
Bae Soo Hyeon,
Hwang Jee Won,
Shin Sang Joon,
Park Gyu Hwan,
Yoon Kee Dong,
Bae Soo Kyung
Publication year - 2013
Publication title -
journal of separation science
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 0.72
H-Index - 102
eISSN - 1615-9314
pISSN - 1615-9306
DOI - 10.1002/jssc.201200779
Subject(s) - chromatography , chemistry , formic acid , mass spectrometry , selected reaction monitoring , pharmacokinetics , tandem mass spectrometry , liquid chromatography–mass spectrometry , analytical chemistry (journal) , high performance liquid chromatography , standard curve , quantitative analysis (chemistry) , matrix (chemical analysis) , medicine
A simple, robust, and rapid LC ‐ MS / MS method was developed for the quantitation of U 0126 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 A gilent P oroshell 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 U 0126 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. U 0126 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 U 0126 at various doses in rats.