Quantitative ionspray liquid chromatographic/tandem mass spectrometric determination of reserpine in equine plasma.
A method based on ionspray liquid chromatography/tandem mass spectrometry (LC/MS/MS) was developed for the determination of reserpine in equine plasma. A comparison was made of the isolation of reserpine from plasma by liquid-liquid extraction and by solid-phase extraction. A structural analog, rescinnamine, was used as the internal standard. The reconstituted extracts were analyzed by ionspray LC/MS/MS in the selected reaction monitoring (SRM) mode. The calibration graph for reserpine extracted from equine plasma obtained using liquid-liquid extraction was linear from 10 to 5000 pg ml-1 and that using solid-phase extraction from 100 to 5000 pg ml-1. The lower level of quantitation (LLQ) using liquid-liquid and solid-phase extraction was 50 and 200 pg ml-1, respectively. The lower level of detection for reserpine by LC/MS/MS was 10 pg ml-1. The intra-assay accuracy did not exceed 13% for liquid-liquid and 12% for solid-phase extraction. The recoveries for the LLQ were 68% for liquid-liquid and 58% for solid-phase extraction.
Anderson
M A
MA
Cornell University, Ithaca, New York 14850, USA.
Wachs
T
T
Henion
J D
JD
D000818:Animals; D002138:Calibration; D002851:Chromatography, High Pressure Liquid; D004300:Doping in Sports; D006736:Horses / Q000097:blood*; D013058:Mass Spectrometry; D015394:Molecular Structure; D012015:Reference Standards; D012110:Reserpine / Q000031:analogs & derivatives / Q000097:blood*
D012110:Reserpine; C084826:rescinnamine