Analysis of saxitixin in urine by continuous‐flow fast‐atom bombardment mass spectromety

Abstract

An improved method of saxitoxin analysis in urine using continuous‐flow fast‐atom bombardment mass spectrometry was developed. Parameters studied were matrix composition, matrix flow, temperature of probe tip, probe‐tip design and sample extraxtion. 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 8μL per min.; probe tip: Olson‐Hogge design. The STX standard was detected at 200pg with signal‐to‐noise ratio of 11. The percent recovery of saxitoxin from human urine after clean‐up on a weak cation exchange column was 75%. Copyright © 1992 John Wiley & Sons, Ltd.