Determination of Cabergoline by Electrospray Ionization Tandem Mass Spectrometry: Picogram Detection via Column Focusing Sample Introduction

Authors

Bruce A. Kimball, USDA/APHIS/WS National Wildlife Research CenterFollow
Thomas J. DeLiberto, USDA/APHIS/WS National Wildlife Research CenterFollow
John J. Johnston, USDA/APHIS/NWRCFollow

Document Type

Article

Date of this Version

October 2001

Comments

Published in Analytical Chemistry, Vol. 73, No. 20, October 15, 2001.

Abstract

An electrospray ionization tandem mass spectrometric method was developed for low-picogram detection of an ergot alkaloid, cabergoline, in coyote plasma extracts. Cabergoline is under investigation as an abortifacient in canid species. Central to the successful development of this method was the ability to introduce relatively large sample volumes into the mass spectrometer. This was achieved by focusing the analyte on a conventional high-performance liquid chromatography guard column prior to elution into the spectrometer. Volumes up to at least 900 μL could be injected onto the guard column using a 100% aqueous mobile phase. Cabergoline retained on the column was eluted as a discreet band into the mass spectrometer by the rapid addition of methanol (30%) to the mobile phase. As compared to flow injection sample introduction, the ability to inject larger sample volumes led to a greatly lowered detection limit. Using this technique and a modification of a previously reported extraction procedure, cabergoline could be determined in coyote plasma at concentrations as low as 9 pg of cabergoline/ mL of plasma.