Determination of Aconitum alkaloids in blood and urine samples. II. Capillary liquid chromatographic-frit fast atom bombardment mass spectrometric analysis.
Determination of fourteen alkaloids, toxic Aconitum alkaloids, aconitine, mesaconitine, jesaconitine, hypaconitine and deoxyaconitine, and their hydrolysis products, benzoylaconines and aconines, have been established using capillary liquid chromatography (LC) fast atom bombardment mass spectrometry (FAB-MS) with a frit interface. Protonated molecular ions were observed as base peaks in the FAB-MS for these fourteen alkaloids. All the alkaloids were simultaneously quantified with linear gradient LC elution by solvent mixture of acetonitrile and 0.3% trifluoroacetic acid using selected ion monitoring of the protonated molecular ions. The calibration curves of these alkaloids were linear in injection amounts ranging from 5 to 500 pg, and their detection limits were 1 pg per injection (S/N=3). Solid-phase extraction using Sep-Pak Plus PS-1 was also investigated to clean-up and concentrate alkaloids in blood and urine samples, and showed satisfactory recoveries. This capillary LC-frit-FAB-MS method enables determination of low levels of Aconitum alkaloids in blood and urine samples, coupled with solid-phase extraction.
National Research Institute of Police Science, Tokyo, Japan.
H
H
Ohta
Y
Y
Seto
N
N
Tsunoda
Y
Y
Takahashi
K
K
Matsuura
K
K
Ogasawara
D000157:Aconitine / Q000031:analogs & derivatives* / Q000097:blood / Q000652:urine; D002851:Chromatography, High Pressure Liquid / Q000379:methods*; D006801:Humans; D006868:Hydrolysis; D016339:Spectrometry, Mass, Fast Atom Bombardment / Q000379:methods*
D000157:Aconitine