Determination of caudatin‐2,6‐dideoxy‐3‐O‐methy‐β‐ d ‐cymaropyranoside in rat plasma using liquid chromatography–tandem mass spectrometry

Abstract A selective, sensitive and rapid liquid chromatography–tandem mass spectrometry method has been developed for the determination of caudatin‐2,6‐dideoxy‐3‐O‐methy‐β‐d‐cymaropyranoside (CDMC) in rat plasma. This method involves a plasma clean‐up step using liquid–liquid extraction, followed by LC separation and positive electrospray ionization mass spectrometry detection (LC/ESI‐MS/MS). Chromatographic separation of the analytes was achieved using a C18 column with a mobile phase of acetonitrile and water (70:30, v/v) at a flow rate of 1.0 mL/min. Low energy collision tandem mass spectrometric analysis (CID‐MS/MS) using the multiple reaction monitoring (MRM) mode was used for analyte quantification. For the MRM analysis of CDMC, the following transition at m/z 658.4 → 529.6 derived from the protonated molecule [M + Na]+. A calibration curve was linear in the 5–500 ng/mL range for CDMC, and the limit of detection was 5 ng/mL. The inter‐ and intra‐day precisions (RSD) were ≤8.5 and ≤9.1%, respectively. The accuracy (RE) was ± 10.9%. The novel developed LC/ESI‐MS/MS method was successfully applied to pharmacokinetic studies of CDMC after oral administration to rats. The total chromatographic run time of this method was 5.0 min per sample, allowing for analysis of a large number of samples per batch. Copyright © 2008 John Wiley & Sons, Ltd.