Yg. Shin et H. Matsuura, Determination of alliin in rat plasma by liquid chromatography-electrospray ionization mass spectrometry, J LIQ CHR R, 23(9), 2000, pp. 1331-1338
A rapid and sensitive high performance liquid chromatography-electrospray/M
S method has been developed to determine alliin in rat plasma. The method i
nvolved deproteinization of these samples with 2.5-volumes (v/w) of acetoni
trile/ethanol (1:1) and then 5 mu L aliquots of the supernatant were inject
ed onto a amino-silica (NH2) column coupled with an electrospray/MS system.
The mobile phase employed isocratic elution with 5% acetonitrile for 10 mi
n; the flow rate was 1.0 mL/min. The column effluent was analyzed by select
ed ion monitoring (SIM) for the negative pseudo-molecular ion of alliin [M-
H](-) at m/z 176. The limit of detection for alliin in rat plasma by this m
ethod was ca. 10 ng/mL and the accuracy for intra- and inter-assay were bet
ween 88.3% and 110.1%. The coefficients of variation of the intra- and inte
r-assay were generally low (below 9.2% and 11.0%, respectively) for rat pla
sma. No problems were encounted due to interference from endogenous substan
ces.