Analysis of Saxitoxin from Urine Using Dynamic FAB/MS.

摘要

An improved method of saxitoxin analysis in urine using continuous Flow Fast Atom Bombardment Mass Spectrometry (CF/FAB/MS) was developed. Parameters studied were matrix composition, matrix flow rate, temperature of probe tip, probe tip design and sample extraction. Optimal detection was obtained using the following matrix composition: 5% glycerol, 0.5% acetic acid, 0.025% sodium dodecylsulfate, 0.1% polyethylene glycol (PEG) 400 and 0.5% PEG 300; probe tip temperature: (-55 C); flow rate: 5 or 8 microliter per min; probe tip: Olson-Hogge design. The STX standard was detected at 200 picograms with signal-to-noise ratio of 11. The percent recovery of saxitoxin from human urine after cleanup on a weak cation exchange (CBA Bond-Elut Analytichem Inter. Varian, Anaheim, CA) column was 75%.