Determination of urinary thiocyanate and nitrate using fast ion-interaction chromatography.
A simple and rapid chromatographic method for determination of nitrite, nitrate and thiocyanate is reported, and applied to the analysis of non-, medium and heavy smokers' urine samples. Ion-interaction liquid chromatography was carried out on a short 30 mm x 4.6 mm C18 column (3 microm particle size) with a mobile phase of 10 mM tetrabutylammonium phosphate in 20% MeOH. The chromatography was performed at an elevated temperature of 45 degrees C, at a flow-rate of 1 ml/min. Detection was by direct UV absorption at 230 nm. Sample preparation involved centrifugation and dilution, followed by sample clean-up on a C18 solid-phase extraction cartridge. The developed method proved both precise (% RSD <2%) and sensitive (standard detection limits <0.1 mg/l), and yielded total run times of under 10 min when applied to urine analysis of smokers and non-smokers, with thiocyanate eluting in under 5 min.
Connolly
Damian
D
National Centre for Sensor Research, School of Chemical Sciences, Dublin City University, Glasnevin, Dublin, Ireland.
Barron
Leon
L
Paull
Brett
B
D002853:Chromatography, Liquid / Q000379:methods*; D006801:Humans; D009566:Nitrates / Q000652:urine*; D015203:Reproducibility of Results; D012907:Smoking / Q000652:urine; D013056:Spectrophotometry, Ultraviolet; D013861:Thiocyanates / Q000652:urine*
D009566:Nitrates; D013861:Thiocyanates